Tag: M.W=300-400

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. 628-21-7, name is 1,4-Diiodobutane, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1,4-Diiodobutane

Stage 1 (0250) An oven-dried 3 L 4-neck flask fitted with an internal thermometer, N2 bubbler, overhead stirrer and oven-dried pressure-equalising dropping funnel was charged with 1,4-dibromo-2,5-dimethylbenzene (70 g, 265 mmol) and dry THF (700 mL). The solution was cooled with stirring to <-70 C. to produce a white slurry. s-Butyllithium (370 mL, 1.4 M, 518 mmol) was charged to the dropping funnel and added dropwise over the space of 2 h ensuring the reaction temperature did not exceed -70 C. The slurry was stirred for 2 h after which GCMS confirmed the lithiation was complete. The dropping funnel was charged with a solution of 1,4-diiodobutane (15.7 mL, 119 mmol) in dry THF (160 mL) which was then added dropwise over 0.75 h. The resulting pale yellow slurry was allowed to warm to room temperature and stirred for 12 h. The reaction was quenched by addition of water. The mixture was transferred to a separating funnel and the layers were separated. The aqueous layer was extracted with diethyl ether and the combined organics were washed with water, dried with MgSO4, filtered and concentrated to yield an off-white solid. The product was triturated with 300 mL methanol for 2 h and recrystallised from toluene/IPA to yield a white powder that was dried in the oven (31.86 g, 63%). GCMS indicated a purity of 96% and the material was taken to the next stage without further purification 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 628-21-7.

Adding a certain compound to certain chemical reactions, such as: 89488-57-3, name is 1,4-Diiodo-2-nitrobenzene, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 89488-57-3, COA of Formula: C6H3I2NO2

(RS)-1-(4-Iodo-2-nitrophenyl)-2,2-dimethyl-1-propanol: Under a nitrogen atmosphere a solution of 1,4-diiodo-2-nitrobenzene (3.0 g, 8.0 mmol) in anhydrous THF (20 mL) was cooled to minus 40 C., and then a solution of phenylmagnesium chloride (2 M in THF, 4.8 mL, 9.6 mmol) was added dropwise at a rate that the temperature would not exceed minus 35 C. Upon completion of the addition the mixture was stirred for ten minutes, followed by addition of trimethylacetaldehyde (1.2 mL, 11.2 mmol), and the mixture was stirred for 30 minutes at minus 40 C. The mixture was gradually warmed up to room temperature, quenched with saturated ammonium chloride (60 mL), poured into water (120 mL), and extracted with ethyl acetate twice (60 mL each). The combined organic phase was washed with water (60 mL), dried over Na2SO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography to yield racemic (RS)-1-(4-iodo-2-nitrophenyl)-2,2-dimethyl-1-propanol (2.17 g, 81%) as a brown oil. 1H NMR (400 MHz, CDCl3): delta 8.04 (d, 1 H, J=1.6 Hz, Ph-H), 7.88 (dd, 1 H, J=1.6 and 8.4 Hz, Ph-H), 7.51 (d, 1 H, J=8.4 Hz, Ph-H), 5.28 (d, 1 H, J=3.6 Hz, Ph-CH), 2.29 (d, 1 H, J=3.6 Hz, OH), 0.85 (s, 9 H, C(CH3)3). 13C NMR (100 MHz, CDCl3): delta 149.87 (C), 141.0 (CH), 136.2 (C), 132.3 (CH), 131.63 (CH), 91.85 (C), 74.33 (CH), 36.81 (C), 25.6 (CH3).

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Electric Literature of 34270-90-1, 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 34270-90-1 as follows.

Preparation of Compounds 1002 – 1005: NaH (28.03 mg, 60%) was added into a solution of 2-(4-fluorophenyl)-5-hydroxy-N-methylbenzofuran-3-carboxamide (50 mg) and (E)-1,4-dibromobut-2-ene (75 mg) inPhH. The reaction was heated at 85C for 4 – 7 days. The reaction was quenched withMeOH and solvents were removed under vaccum to give a residue which was purified bypreparative HPLC._Compounds 1003 – 1015 and 2001 – 2005 were prepared using the sameprocedure for compound 1002, using the corresponding di-electrophiles. LC condition for compounds 1003 – 1015 and 2001 – 2005 was the same as for compound 1002.

According to the analysis of related databases, 34270-90-1, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 3268-21-1, name is 1,4-Diiodo-2,3,5,6-tetramethylbenzene, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 3268-21-1, Safety of 1,4-Diiodo-2,3,5,6-tetramethylbenzene

To a solution of 1 (3.02 g, 7.82 mmol, 1 equiv), Pd(PPh3)2Cl2 (0.380 g, 0.541 mmol, 0.07 equiv) and CuI (0.101 g, 0.530 mmol, 0.07 equiv) in Et2NH was added ethynyltrimethylsilane (2.45 mL, 17.3 mmol, 2.2 equiv) and the reaction was stirred at RT overnight. The solvent was evaporated followed by extraction with CH2Cl2 (3 >< 100 mL) and washing of the organic layer with H20 (2 >< 200 mL) and brine (250 mL). The combined organic layers were dried over MgSO4 and concentrated in vacuo. The product was (0279) purified via column chromatography (PE) leading to 2 as off-white crystals (82%). 1H NMR (400 MHZ, CDClg) 6 2.38 (s, 12H), 0.27 (s, 18H). 13C NMR (400 MHZ, CDC13)8 136.0, 123.4, 104.2, 103.2, 18.5, 0.27. IRV 2957, 2138, 1270, 1073, 863 cm-1. HRMS (EI+) m/z caIcuIated for C20H30Si2 326.1886, found 326.1870. If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

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. 6326-42-7, name is Methyl 2-iodo-4-nitrobenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 6326-42-7

A solution of the compound 8 (10.0 g, 32.57 mmol) and SnCl2. 2 hi) (22.04 g, 97,69 mmol, 3 equiv.) in EtOAc ( 150 mL) was refluxed for 5 hours until TLC (EtOAc/hexane, 1 : 1) indicated that reaction was complete. The reaction mixture was poured in a 500 ml beaker and it was diluted with 100 ml of EtOAc followed by the addition of potassium carbonate and 200 ml of deionized water and the two layer mixture was stirred for 30 minutes. The milky suspension was filtered through a short bed of CELITE and the organic layer was separated. The combined organic layer was sequentially treated with saturated brine and anhydrous Na2S0 . Purification by flash column chromatography using EtOAc: petroleum ether (1 : 1) afforded a pale yellow solid 9 (5.86 g, 65% yield). [0396] FontWeight=”Bold” FontSize=”10″ 1I NMR (400 MHz, CDC13, TMS) delta 3.86 (s, 3H), 4.01 (broad singlet, 2H), 6.58-6.64 (dd, IH, Jj = 2.29 Hz, J2 = 8.70 Hz), 7.30 (d, 1H, J = 2.29 Hz), 7.77 (d, 1H, J – 8.24 Hz). 1 C NMR (100 MHz, CDC13) delta: 51.87, 96.53, 1 13,44, 127,03, 132.95, 150,24, 165,92, MS (ESI): m/z (%) 300. 9 (M Xa }

The synthetic route of 6326-42-7 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 175278-11-2, A common heterocyclic compound, 175278-11-2, name is 1-Bromo-3,5-difluoro-2-iodobenzene, molecular formula is C6H2BrF2I, 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.

To a cooled solution of l-bromo-3,5-difluoro-2-iodobenzene (10.0 g, 31.4 mmol) in THF (25 mL, 1.3 M) at -20 C was added a solution of iPrMgCl (2M in THF, 20.4 mL, 40.8 mmol) dropwise. The mixture was stirred for 10 min and then warmed to 0 C and stirred an additional 50 min. Copper iodide (1.49 g, 7.84 mmol) was added, and the mixture was stirred for 10 min. Ethyl 2-(bromomethyl)acrylate (6.36 g, 4.55 mL, 32.9 mmol) was added, and the mixture was warmed to room temperature and stirred overnight. The reaction was quenched with sat. aq. NH4C1 (25 mL), diluted with EtOAc (25 mL) and extracted with EtOAc (3 x 30 mL). The combined organics were washed with brine (4 x 50 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The resulting residue was purified by silica gel column to give the desired product l-bromo- 3,5-difluoro-2-(2-methylallyl)benzene as a colorless and clear oil (10 g). Yield >95%.

The synthetic route of 175278-11-2 has been constantly updated, and we look forward to future research findings.

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. 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid

EXAMPLE 6 1-F3, 4-DIFLUORO-2- (2-FLUORO-4-VINVIPHENYLAMINO)-PHENVLL-2-HYDROXV-ETHANONE Step A: Synthesis of R3, 4-DIFLUORO-2- (2-FLUORO-4-IODOD-PHENYLAMINO)-PHENVLL- methanol. To 3, 4-DIFLUORO-2-(2-FLUORO-4-IODO-PHENYLAMINO)-BENZOIC acid (10. 0g, 25. 4MMOL) in tetrahydrofuran was added, borane in tetrahydrofuran (38.2mL of a 1. OM solution) after 16 hours stirring at room temperature, the reaction was complete and quenched by careful addition of 2% HCI (100ML). The mixture was stirred for 1 H, brine was added and the organic layer was separated which was dried and evaporated to give a colorless solid (7. 13g 74%) that was recrystalized from hot dichloromethane/hexane to give an analytical sample. MS (APCI+) 380 (M+1+) ; H NMR (400mHz, DMSO) 7.62 (s, 1H), 7.50 (d, 1H), 7.24 (m, 3H), 6.29 (d of t, 1 H), 5.35 (t, 1 H), 4.42 (d, 1 H).

According to the analysis of related databases, 391211-97-5, the application of this compound in the production field has become more and more popular.

Application of 260355-20-2,Some common heterocyclic compound, 260355-20-2, name is 1-Chloro-4-iodo-2-(trifluoromethyl)benzene, molecular formula is C7H3ClF3I, 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.

The 1-chloro-4-iodo-2-trifluoromethylbenzene (10 mmol) obtained in the reaction 1.2 was dissolved in 20 ml of toluene, and the system was sequentially added with isoxazol-4-amine (12 mmol), palladium acetate ( 0.5 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (12 mmol), 3 ml of triethylamine. After stirring for 10 minutes, add 10 ml of cesium carbonate (10 mmol). The aqueous solution is heated to 50 C for 4 hours. After the reaction is completed, 20 ml of water is added to the system, stirred for 20 minutes, and the organic phase is dried over anhydrous sodium sulfate, concentrated, and then purified by flash column chromatography.2.2 g of yellow N-(4-chloro-3-trifluoromethylphenyl)-isoxazole-4-amine powder was obtained in a yield of 84%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Chloro-4-iodo-2-(trifluoromethyl)benzene, its application will become more common.

Electric Literature of 628-77-3,Some common heterocyclic compound, 628-77-3, name is 1,5-Diiodopentane, molecular formula is C5H10I2, 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.

Sodium hydride (9.73 mg, 0.243 mmol, 60%> suspension in mineral oil) was added to a solution of l ,3-difluoro-2-(((l ,l ,l ,3,3,3-hexafluoro-2-(4-(((4- fluorophenyl)sulfonyl)methyl)phenyl)propan-2-yl)oxy)methyl)benzene (13.2 mg, 0.024 mmol) and 1 ,5-diiodopentane (31.5 mg, 0.097 mmol) in Nu,Nu-dimethylformamide (1 mL). After 1 h at room temperature, LCMS analysis showed that the reaction was complete. The mixture was quenched with water (1 mL), diluted with ether (10 mL), washed with water (2×10 mL), brine (5 mL), dried (magnesium sulfate), filtered and concentrated under reduced pressure. The crude material was purified via preparative LC/MS with the following conditions: Column: Waters XBridge C18, 19 x 150 mm, 5-muiotaeta particles; Guard Column: Waters XBridge C I 8, 19 x 10 mm, 5-muiotaeta particles; Mobile Phase A: 5 :95 acetonitrile: water with 10-mM ammonium acetate; Mobile Phase B: 95 :5 acetonitrile: water with 10-mM ammonium acetate; Gradient: 60-100% B over 15 minutes, then a 5-minute hold at 100% B; Flow: 20 mL/min. Fractions containing the desired product were combined and dried via centrifugal evaporation to give Example 1 (9.0 mg, 57% yield). LC/MS (M+18): 628.1 ; LC retention time: 3.130 min (analytical HPLC Method C); 1H NMR (500 MHz, 1 : 1 mixture of CDC13-CD30D) delta ppm 7.66 – 7.58 (m, 2H), 7.49 – 7.38 (m, 3H), 7.30 – 7.21 (m, 2H), 7.08 – 6.95 (m, 4H), 4.73 (s, 2H), 2.66 (d, J=12.9 Hz, 2H), 2.26 (td, J=13.3, 3.2 Hz, 2H), 1.83 (d, J=13.4 Hz, 2H), 1.67 (d, J=12.4 Hz, 1H), 1.47 – 1.34 (m, 1H), 1.28 (q, J=13.0 Hz, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,5-Diiodopentane, its application will become more common.

These common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, 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. Formula: C8H6BrIO2

Synthesis of Intermediate 1-(6) (0202)3.849 g (11.259 mmol) of methyl 5-bromo-2-iodobenzoate, 3 g (13.510 mmol) of Intermediate 1-(6) (phenanthren-1-ylboronic acid), 30 mL of 2 mol/L potassium carbonate in H2O, and 0.651 g (0.563 mmol) of tetrakis(triphenylphosphine)palladium were added to 100 mL of tetrahydrofuran and 30 mL of methanol under a nitrogen atmosphere and then heat-stirred. After 24 hours, completion of the reaction was confirmed through TLC, and the solvent was removed and filtered using celite. Next, the organic layer was separated using dichloromethane and H2O and washed with a saturated sodium chloride solution. The organic layer was dried with sodium sulfate and filtered. After drying and filtering, the solvent was removed and column chromatography (MC:hexane=1:4) was performed to obtain 3.5 g of Intermediate 1-(6) as a white solid (yield: 79%). (0203) 1H NMR (300 MHz, CDCl3): delta (ppm) 8.80 (d, J=12.6 Hz, 2H), 8.22 (s, 1H), 7.88 (d, J=7.8 Hz, 1H), 7.77 (dd, J=5.1, 1.8 Hz, 1H), 7.737.60 (m, 4H), 7.40 (dd, J=7.8, 1.5 Hz, 2H), 7.32 (d, J=8.1 Hz, 1H), 3.41 (s, 3H) (0204) 13C NMR (75 MHz, CDCl3): delta (ppm) 166.4, 140.7, 139.0, 134.6, 133.5, 133.1, 131.7, 130.3, 130.2, 130.0, 128.5, 127.2, 126.8, 126.7, 125.7, 123.9, 122.9, 122.4, 121.5, 52.1 (0205) A molecular weight for C22H15BrO2: Cal. 390.0255 (0206) LR-Mass (EI+): 392.2, HR-Mass (EI+): 392.0257

The synthetic route of Methyl 5-bromo-2-iodobenzoate has been constantly updated, and we look forward to future research findings.