Month: May 2021

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 624-76-0, name is 2-Iodoethanol, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Iodoethanol

[00396] To a jacketed glass reactor equipped with overhead stirring, was charged tert-butyl ((2R,3R,4R,5R)-2-(((l S,2S,3R,4S,6R)-3-(((2S,3R)-6-(aminomethyl)-3-((tert- butoxycarbonyl)amino)-3,4-dihydro-2H-pyran-2-yl)oxy)-4-((tert-butoxycarbonyl)amino)-6- ((S)-4-((tert-butoxycarbonyl)amino)-2-hydroxybutanamido)-2-hydroxycyclohexyl)oxy)-3,5- dihydroxy-5-methyltetrahydro-2H-pyran-4-yl)(methyl)carbamate, formula (6a), (250 g, 0.263 mol, 1 equiv). Acetonitrile (1250 mL) was charged to the reactor and the temperature was stabilized between 15 and 30 C (24.3 C). The mixture was concentrated under vacuum to a final volume target of 500 mL. The solution was sampled for water content by KF which provided a result of 0.22% w/w. An additional portion of acetonitrile (750 mL) was charged to the reactor and a second azeotropic distillation was performed to a volume target of 500 mL. The mixture was sampled for KF and a result of 0.097%> w/w was obtained. The reaction temperature was stabilized at 29.9 C and acetone (1250 mL) was charged to the mixture. The reaction was heated and the temperature stabilized at 29.9 C. Sodium bicarbonate (44.25 g, 0.527, 2.0 equiv) was charged to the reaction mixture followed by 2-iodoethanol (44.4 g, 20.14 mL, 0.258 mol, 0.98 equiv). After 43 h an additional portion of 2-iodoethanol (0.25 mL) was added to the reaction mixture. After 9.5 hours a third portion of 2-iodoethanol (0.3 mL) was added to the reaction mixture. After an additional 2 h, the reaction was sampled and deemed complete by HPLC analysis (consumption of tert-butyl ((2R,3R,4R,5R)-2- (((l S,2S,3R,4S,6R)-3-(((2S,3R)-6-(aminomethyl)-3-((tert-butoxycarbonyl)amino)-3,4- dihydro-2H-pyran-2-yl)oxy)-4-((tert-butoxycarbonyl)amino)-6-((S)-4-((tert- butoxycarbonyl)amino)-2-hydroxybutanamido)-2-hydroxycyclohexyl)oxy)-3,5-dihydroxy-5- methyltetrahydro-2H-pyran-4-yl)(methyl)carbamate, formula (6a),). The reaction was cooled to 22.7 C and l,4-diazabicyclo[2.2.2]octane (60.0 g, 0.535 mol, 2.03 equiv) was charged as a solid. The destruction of 2-iodoethanol was monitored by a GC method and after 10 h the quench of this reagent was deemed complete. Water (1250 mL) and isopropyl acetate (1250 mL) were charged to the reaction mixture. The reactor contents were agitated by 25 min and the layers allowed to separate. The lower aqueous layer (API) and the upper organic layer (OP1) were collected in receivers. API was returned to the reactor and a second portion of isopropyl acetate (750 mL) was charged. The reactor contents were agitated for 30 minutes and the layers allowed to separate. The lower aqueous layer (AP2) and the upper organic layer (OP2) were collected in receivers. OP1 and OP2 were combined in the reactor and extracted with two portions of saturated sodium chloride solution (750 mL, prepared by dissolving 100 g NaCl/290 mL of water). The washed organic phase (OP4) was concentrated under vacuum to a volume target of 500 mL. Acetonitrile (2550 mL) was charged to the reactor. A second azeotropic vacuum distillation was performed to a volume target of 1550 mL. Isopropyl acetate (200 mL) was charged to the mixture. Water (10.7 mL) was charged to the mixture until a KF of 0.85% was obtained. The reactor contents were heated to 75 C upon which a solution was obtained. The reaction mixture was cooled to 57 C and seeded with tert-butyl ((2R,3R,4R,5R)-2-(((l S,2S,3R,4S,6R)-4-((tert-butoxycarbonyl)amino)-6-((S)- 4-((tert-butoxycarbonyl)amino)-2-hydroxybutanamido)-3-(((2S,3R)-3-((tert- butoxycarbonyl)amino)-6-(((2-hydroxyethyl)amino)methyl)-3,4-dihydro-2H-pyran-2- yl)oxy)-2-hydroxycyclohexyl)oxy)-3,5-dihydroxy-5-methyltetrahydro-2H-pyran-4- yl)(methyl)carbamate, formula (7a), (5 g, 0.0050 mol, 0.02 equiv). Stirring was maintained at 57 C for 2 h during which a thick slurry formed. The mixture was cooled from 65 C to 2.5 C over a period of 12 h. The slurry was filtered and washed with acetonitrile (900 mL) and dried in a vacuum oven to afford tert-butyl ((2R,3R,4R,5R)-2-(((l S,2S,3R,4S,6R)-4-((tert- butoxycarbonyl)amino)-6-((S)-4-((tert-butoxycarbonyl)amino)-2-hydroxybutanamido)-3- (((2S,3R)-3-((tert-butoxycarbonyl)amino)-6-(((2-hydroxyethyl)amino)methyl)-3,4-dihydro- 2H-pyran-2-yl)oxy)-2-hydroxycyclohexyl)oxy)-3,5-dihydroxy-5-methyltetrahydro-2H-pyran- 4-yl)(methyl)carbamate, formula (7a), (218.1 g, 0.220 mol, 83% molar yield)

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 624-76-0.

Electric Literature of 31599-60-7, The chemical industry reduces the impact on the environment during synthesis 31599-60-7, name is 1-Iodo-2,3-dimethylbenzene, I believe this compound will play a more active role in future production and life.

1-(bromomethyl)-3-iodo-2-methylbenzole 1-iodo-2,3-dimethylbenzole (0.7 mL, 5.0 mmol) and N-bromosuccinimide (890 mg, 5.0 mmol) were dissolved in 1,2-dichloroethane (10 mL), then 2,2′-azobisisobutyronitrile (16 mg, 0.1 mmol, 2 mol %) was added and the solution refluxed 2 h. After the reaction mixture had cooled to RT, it was diluted with 1,2-dichloroethane (40 mL) and washed with water (2*50 mL). The organic phase was dried (MgSO4) and evaporated to low bulk and used in the following synthesis step. (Yield: 9.2 g, 72%)

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Iodo-2,3-dimethylbenzene, other downstream synthetic routes, hurry up and to see.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 450412-29-0, name is 1-Bromo-3-fluoro-2-iodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Bromo-3-fluoro-2-iodobenzene

200 g (664 mmol) of 1-bromo-3-fluoro-2-iodobenzene, 101 g (664 mmol) of 2-methoxyphenylboronic acid and 137.5 g (997 mmol) of sodium tetraborate are dissolved in 1000 ml of THF and 600 ml of water, and degassed. 9.3 g (13.3 mmol) of bis(triphenylphosphine)palladium(II) chloride and 1 g (20 mmol) of hydrazinium hydroxide are added. The reaction mixture is stirred under a protective gas atmosphere at 70 C. for 48 h. The cooled solution is supplemented with toluene, washed repeatedly with water, dried and concentrated. The product is purified via column chromatography on silica gel with toluene/ heptane (1:2). Yield: 155 g (553 mmol), 83% of theory.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 491862-84-1, name is 3-Fluoro-5-iodotoluene, A new synthetic method of this compound is introduced below., Product Details of 491862-84-1

[00464j To a 1OOml flask was added 3-bromo-1H-i,2,4-triazole (739.8 mg, 5 mmol), CuT (95.2 mg, 0.50 mmol) and Cs2C03 (1.629 g, 5.0 mmol) and the flask was evacuated thenbackfilled with N2 before adding DMS0 (5 mL) and i-fluoro-3-iodo-5-methyl-benzene (590.1 mg, 2.50 mmol). The reaction mixture was heated at 100C for 20h at which time LCMSindicated the major peak was desired product. To the reaction mixture was added Et0Ac, the mixture was filtered through celite and to the filtrate was added brine. The organic phase wasdried over MgS04, filtered, evaporated to dryness and purified on an Isco 40g silica gel column eluting with heptanes and ethyl acetate to afford 3-bromo-i-(3-fluoro-5-methyl-phenyl)-i,2,4-triazole HG-3a (170 mg, 26.6%). ?H NMR (300 MHz, CDC13) oe 8.43 (s, 1H), 7.29 (d, J = 2.7 Hz, 1H), 7.23 (dt, J = 9.0, 2.0 Hz, 1H), 6.97 (d, J = 9.1 Hz, 1H), 2.46 (s, 3H)ppm. ESI-MS m/z calc. 254.98074, found 257.97 (M+i) Retention time: 0.81 minutes.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 17024-12-3, name is 9-Iodophenanthrene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 17024-12-3

General procedure: A 25 mM solution of iodobenzene (5a) and K2CO3 (2 equiv) in H2O/CH3CN (2:1) was pumped at a flow rate of 1.0 mL/min(contact time: 58 s) through a Phoenix flow reactor systemequipped with two cartridges of 4 (total 500 mg; 0.084 mmolPd). Flow hydroxycarbonylation with CO gas introduced from agas module (10 mL/min) was conducted at 100 C and a systempressure of 5 bar. The resulting solution was collected for 50min (50 mL) and the solvent was removed by evaporation. 2 Naq HCl (10 mL) was added and the resulting solid was collectedby filtration, washed with H2O (3 × 10 mL), and dried undervacuum to give benzoic acid (9a) as a white solid without anyfurther purification.Yield: 125 mg (82%); mp 122 C; 1H NMR(400 MHz, DMSO-d6): delta = 12.96 (br s, 1 H, COOH), 7.93 (d, J = 7.2Hz, 2 H, PhH-2 and PhH-6), 7.62 (t, J = 7.2 Hz, 1 H, PhH-4), 7.49 (t, J =7.2 Hz, 2 H, PhH-3 and PhH-5); 13C NMR (101 MHz, DMSO-d6): delta = 167.32 (COOH), 132.87 (Ph), 130.76 (Ph), 129.26 (Ph),128.57 (Ph); ESI-TOF-MS (neg.): m/z = 121 [M – H]-.

According to the analysis of related databases, 17024-12-3, the application of this compound in the production field has become more and more popular.

Related Products of 364-12-5, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 364-12-5 as follows.

Step 1: 1-(4-bromo-2-(trifluoromethyl)phenyl)ethanone MS: 266.9 [M++1]

According to the analysis of related databases, 364-12-5, the application of this compound in the production field has become more and more popular.

Electric Literature of 886762-73-8, The chemical industry reduces the impact on the environment during synthesis 886762-73-8, name is 2-Fluoro-6-iodoaniline, I believe this compound will play a more active role in future production and life.

3.90.2. Step ii): 2-ethyl-6-fluoroaniline PdCl2dppf (0.1 eq, 375 mg), Cs2C03 (3 eq, 4.5 g) and 6-fluoro-2-iodoaniline (1 eq, 1.1 g) are dissolved in dry DMF (50 mL) in a 250 mL round bottom flask. The suspension is degassed under nitrogen atmosphere for 10 min, followed by the addition of triethylborane (1M in hexane, 1.3 eq, 6.0 mL). The reaction is heated to 55C for 2 h, using a condenser. Upon completion of the reaction, as shown by LC-MS, the suspension is filtered over a Celite pad, which is washed with DCM. The filtrate is poured into water and extraction with DCM (3 x 50 mL) is performed. The combined organic layers are dried (Na2S04) and concentrated in vacuo. The residue is purified by silica chromatography (petroleum ether/EtOAc; 100:0 to 80:20) to give the desired product.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Fluoro-6-iodoaniline, other downstream synthetic routes, hurry up and to see.

Application of 619-58-9, The chemical industry reduces the impact on the environment during synthesis 619-58-9, name is 4-Iodobenzoic acid, I believe this compound will play a more active role in future production and life.

EXAMPLE 10: (E)-3- [4- (8, 8-Dimethyl-5-p-tolyl-7,8- dihydro-2-naphthylselanyl) phenyl] acrylic acid a. 2-(4-IODOPHENYL) ETHANOL 12.5 g (50.4 mmol) of 4-iodobenzoic acid are dissolved in 125 ml of. tetrahydrofuran, and 112 ml (122 mmol) of a 1M solution of borane in tetrahydrofuran are then added dropwise. The reaction medium is stirred for 4 hours, acidified with 2N hydrochloric acid solution and then extracted with ethyl acetate. A white solid is obtained (11.49 g ; yield = 97%).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 41252-95-3 as follows. SDS of cas: 41252-95-3

To a jacketed reactor, N,N-dimethylacetamide (DMAc) (120 mL) and soium ethylate (NaOEt) powder (12.1 g) is charged at 20 C. Diethylmalonate (28.8 g) is added dropwise into the above mixture while keeping internal temperature at around 10 C. After finishing addition, warm up the mixture to 20 C, and continue to stir for another 10 minutes. Then, 2-chloro-5- iodonitrobenzene (17 g) is added in one portion, and heat the mixture to 78 C and stir for usually at least 2.5 hours until process monitor shows almost complete conversion. The resulting mixture is cooled down to 20 C, and it is quenched by 2 N cold aq. HCI solution (180 mL). The bottom yellow oil was tranfered to a jaceket reactor with ethanol (92 mL) in it. Then, to the above solution the first portion of SnCI2.2H20 (30 g) powder is added, and the resulting mix- ture is heated to 70 C and stirred for 1 hour. The second portion of SnCI2.2H20 (30 g) is added, the mixture is stirred usually at least 0.5 hour until process monitor shows almost complete conversion. Then, heat the resulting mixture to 80 C and add 36% aq. HCI solution (60 mL) during 0.5 hour. The mixture is stirred for at least 2.5 hours until process monitor shows almost complete conversion. Then, to the mixture water (90 mL) is added and the resulting mix- ture is cooled down to 20 C. Collect the solid by filtration and wash the solid with water (250 mL) to afford the crude 6-iodo-2-oxindole. Then, it is purified by crystallization with acetic acid (HOAc) (1 10 mL), and followed by washing with 3 N aq. HCI solution (80 mL) to afford the 6- iodo-2-oxindole in 53% yield and 99% HPLC purity (Rt = 7.45 min).

According to the analysis of related databases, 41252-95-3, the application of this compound in the production field has become more and more popular.

Electric Literature of 5876-51-7, A common heterocyclic compound, 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, molecular formula is C7H5IO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

[00233] To 24.7 mg PdCl2[(PPh2(CH2)5PPh2] in a reaction tube under nitrogen was added 4 ml dioxane and 0.43 ml (3.0 mmol) of triethylamine. The mixture was heated at 80 C. to give an orange coloured solution which still contained solids, presumably PdCl2[(PPh2(CH2)5PPh2]. To this mixture, at room temperature, were added 0.23 ml (1.5 mmol) pinacolborane (solution became brown but still contained insolubles) and 255 mg (1.03 mmol) 1-iodo-3,4-methylenedioxybenzene. The reaction solution was warmed to 80 C. with stirring in an oil bath. Analysis of the reaction solution by gc, as described above, was carried out at intervals (see Table 20.1). The reaction was complete after 5 h reaction time. The reaction solution was a bright crimson colour at the completion of the reaction and the only solids present on cooling to room temp. appeared to be the triethylamine salt. The amount of pinacol ester of phenylboronic acid formed is low with PdCl2[(PPh2(CH2)5PPh2] as catalyst and forms only later in the reaction. [TABLE-US-00009] TABLE 20.1 Rate of product formation on reaction of 1-iodo-3,4-methylenedioxybenzene with pinacolborane at 80 C. The catalyst PdCl2[(PPh2(CH2)5PPh2] was heated with the base triethylamine (3.0 mmol) prior to reaction. The concentrations are expressed in area % (uncorrected for response factors) determined by gc analysis of aliquots of the reaction solution taken at selected reaction times*. Reaction Time (mins) [C00056] [C00057] [C00058] [C00059] 5 0 0 99 1 15 0 0 90 10 30 4.0 0 60 36 60 5.2 0 40 54 150 7.1 1.8 13 78 210 7.9 2.1 3.5 86 300 9.3 2.4 0 88 *The reaction was quenched at the selected reaction time by addition of the aliquot of reaction solution to a water/ethyl acetate mixture.

The synthetic route of 5876-51-7 has been constantly updated, and we look forward to future research findings.