Iodides-buliding-blocks

Reference of 123158-75-8, 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 123158-75-8 as follows.

b) To a solution of 4-chloro-2-iodo-5-nitroaniline (8.5 g) in ethanol (38 ml) was added concentrated sulphuric acid (4.4 ml) dropwise, then the solution was heated to reflux and solid sodium nitrite (4.9 g) added in small amounts over 30 minutes. The mixture was refluxed a further one hour and poured into ice water, the product extracted into ethyl acetate, washed with water and brine and the organic layer was dried over sodium sulfate. The solution was evaporated and the residue purified by column chromatography to give 5-chloro-3-iodonitrobenzene (3.4 g). delta (360 MHz, DMSO-d6) 8.28 (1H, d, 2-H), 8.35 (1H, d, 6-H) and 8.46 (1H, d, 4-H).

According to the analysis of related databases, 123158-75-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Merck Sharp & Dohme Limited; US5270309; (1993); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 645-00-1,Some common heterocyclic compound, 645-00-1, name is 1-Iodo-3-nitrobenzene, molecular formula is C6H4INO2, 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.

General procedure: Condition B: An oven-dried pressure tube (10 mL) was charged with sodium sulfide nonahydrate (144 mg, 0.6 mmol), acetic acid (36 mg, 0.6 mmol), nitrobenzene (24.6 mg, 0.2 mmol), DMF (0.8 mL). The reaction vessel was closed under air and the resulting solution was stirred at room temperature for 20 h. Then the reaction mixture was filtered through a pad of silica gel and washed with 5 mL ethyl acetate for three times. The filtrate was removed under vacuum and the residue was purified by flash column chromatography (silica gel, petroleum ether/ethyl acetate = 4:1) to give the desired product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Iodo-3-nitrobenzene, its application will become more common.

Reference:
Article; Shuai, Qi; Li, Jun; Zhao, Feng; Su, Weike; Deng, Guojun; Chemical Papers; vol. 73; 4; (2019); p. 965 – 975;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 624-75-9, These common heterocyclic compound, 624-75-9, name is 2-Iodoacetonitrile, 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.

General procedure: Starting amine (5.0 mmol) was dissolved in dry diethyl ether (17 mL) and iodoacetonitrile (5.5 mmol, 919 mg) was added dropwise under cooling. The mixture was stirred at room temperature for 3-14 days, then precipitate was filtered off, washed with diethyl ether and dried in vacuo to give the corresponding quaternary ammonium salt 2. If the solid precipitate was not formed after 7 days, the mixture was evaporated under reduced pressure. The crude product was washed with diethyl ether (3 × 15mL) and dried in vacuo. The quaternary ammonium salt 2 was used in the next step without additional purification. The corresponding quaternary ammonium salt (3.0 mmol) was heated at 150 C on oil bath in freshly distilled DMF (7 mL) in a 25 mL round-bottom flask fitted with reflux condenser and CaCl2-tube for 15 minutes. The mixture was cooled to room temperature, diluted with H2O (20 mL) and extracted with PhMe (2 × 15mL). The organic phase then was washed with H2O (2 × 15mL) and brine (15 mL), dried over Na2SO4 and evaporated in vacuo to give the desired aminoacetonitrile 4. The latter, if necessary, was purified by column chromatography (it is convenient to visualize aminoacetonitriles on TLC-plate by treating with the diluted solution of ninhydrin in EtOH). Note, that aminoacetonitriles are moisture sensitive. Products after column chromatography were additionally dried by the addition of dry PhMe (5 mL) and evaporation in vacuo.

Statistics shows that 2-Iodoacetonitrile is playing an increasingly important role. we look forward to future research findings about 624-75-9.

Reference:
Article; Buev, Evgeny M.; Smorodina, Anastasia A.; Stepanov, Maxim A.; Moshkin, Vladimir S.; Sosnovskikh, Vyacheslav Y.; Tetrahedron Letters; vol. 59; 17; (2018); p. 1638 – 1641;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

82998-57-0, name is 3-Iodo-4-methylbenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C8H7IO2

Compound 5.3. Methyl 3-iodo-4-methylbenzoate. To a solution of 3-iodo-4- methylbenzoic acid (28.0 g, 0.107 mol) in MeOH (300 mL) at 0 C was carefully added concentrated H2SO4 (30 mL). The mixture was heated at 60 C overnight, then cooled and the solvent removed under reduced pressure. The residue was carefully poured onto ice-water (200 mL) and the mixture was extracted with EtOAc (500 mL). The organics was washed with water (100 mL), saturated NaHC03 (100 mL), brine (100 mL), dried (MgS04), filtered, and concentrated to yield the title compound as a brown oil (29.0 g, 98%). XH NMR (400 MHz, CDCI3) delta 8.47 (d, J= 1.7 Hz, 1H), 7.90 (dd, J= 7.9 Hz, 1.7 Hz, 1H), 7.29 (d, J= 7.9 Hz , 1H), 3.90 (s, 2H), 2.48 (s, 3H)

The synthetic route of 82998-57-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; 3-V BIOSCIENCES, INC.; HEUER, Timothy Sean; OSLOB, Johan D.; MCDOWELL, Robert S.; JOHNSON, Russell; YANG, Hanbiao; EVANCHIK, Marc; ZAHARIA, Cristiana A.; CAI, Haiying; HU, Lily W.; WO2015/95767; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 19718-49-1, 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. 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

INTERMEDIATE 42 Methyl 3-{[(3^-4-(tert-butoxycarbonvnmorpholin-3-yl1methvU-2-ftrimethylsilyl’)-l//- intlupsilonle-5-earbupsilonxyldleTo a stirred solution of Intermediate 41 (31.9 g, 107.4 mmol) in DMF (160 mL) was added methyl 4-amino-3-iodobenzoate (29.8 g, 107.4 mmol), lithium chloride (4.5 g, 107.4 mmol) and sodium carbonate (22.8 g, 214.8 mmol). The resulting suspension was degassed before addition of palladium acetate (0.96 g, 4.3 mmol). The reaction mixture was heated to 11O0C for 50 minutes. It was cooled to r.t, filtered through celite, and concentrated in vacuo. The resulting brown oil was partitioned between isopropyl acetate and water (150 mL each). The aqueous fraction was extracted with isopropyl acetate (2 x 15OmL). The combined organic fractions were dried (MgSO4), treated with decolourising charcoal (5% by weight of crude material) for 30 minutes at room temperature, concentrated in vacuo and then purified by column chromatography (SiO2, DCM) to give the title compound (9g, 19%) as a pale cream solid. LCMS (ES+) 469.1 (M+ Na), RT 4.62 minutes {Method ).

The chemical industry reduces the impact on the environment during synthesis Methyl 4-amino-3-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; UCB PHARMA S.A.; WO2009/71895; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 52548-14-8, 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 52548-14-8 as follows.

A solution of 2-iodo-5-methylbenzoic acid (4.0 g, 15.3 mmol) in DMF (10 mL) was treated with 1,2,3-triazole (2.1 g, 30.5 mmol), Cs2CO3 (9.95 g, 30.5 mmol), CuI (0.145 g, 0.76 mmol) and trans-N,N’-dimethylcyclohexane-l,2-diamine (0.43 g, 3.05 mmol). The mixture was heated at 120 0C for 10 min in a microwave reactor. The reaction was cooled to room temperature, diluted with water, and washed with EtOAc. The aqueous phase was acidified with IN HCl and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by gradient elution on SiO2 (0 to 10% MeOH in DCM with 0.1% AcOH) to give the faster eluting 2-(2H-l,2,3-triazol-2-yl)-5-methylbenzoic acid A-5, followed by the undesired regioisomer isomer, l-(2H-l,2,3-triazol-2-yl)-5-methylbenzoic acid. Data for A-5: 1HNMR (500 MHz, DMSO-d6) d 12.98 (br s , IH), 8.04 (s, 2H), 7.72-7.45 (m, 3H), 2.41 (s, 3H) ppm.

According to the analysis of related databases, 52548-14-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK SHARP & DOHME CORP.; COX, Christopher, D.; COLEMAN, Paul, J.; SCHREIER, John, D.; WO2010/48014; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, A new synthetic method of this compound is introduced below., Application In Synthesis of 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide

In a three-necked flask equipped with a stirrer and a reflux condenser,5-amino-N, N’-bis- (2,3-dihydroxypropyl) -2,4,6-triiodo-1,3-benzenedicarboxamide (84.6 g, 0.12 mol)N, N-dimethylacetamide (172 ml)Stir,Heated to 50 C dissolved, cooled to 10 C,A solution of chloroacetyl chloride (62 ml, 88.09 g, 0.78 mol)About 30min drop finished,The temperature was raised to 50 C for 3 h,Cooling to 0 ~ 10 ,At 10 ,Dropping 10 ml / L of sodium hydroxide solution 156 ml,Stir at room temperature for 1 h.After adding 100 ml of water, 59 ml of 1N hydrochloric acid was added dropwise, and the mixture was allowed to stand overnight. The filtrate was washed with water and dried to give 83.2 g of a yield of 90.0%.

The synthetic route of 76801-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiang Su Heng Rui Medicine Co., Ltd.; Hou, Xianshan; Wang, Junyan; Wang, Zhian; Zhong, Xinguang; (9 pag.)CN106278929; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 51628-12-7,Some common heterocyclic compound, 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile, molecular formula is C8H6IN, 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.

EXAMPLE 10 alpha-cyano-4-iodo-2′,4′,5′-trimethoxystilbene was obtained in the same method as in Referential Example 1 except that 392 mg (2.0 mmol) of 2,4,5-trimethoxybenzaldehyde (purchased from Lancaster) and 486 mg (2.0 mmol) of 4-iodophenylacetonitrile instead of 4-bromophenylacetonitrile were used. 4-iodophenylacetonitrile was obtained in the same method described in Referential Example 3. And 566 mg (yield: 74.4%) of the compound as a yellow crystalline represented by the following formula was obtained in the same method as in Example 1 except that 421 mg (1.0 mmol) of the above alpha-cyano-4-iodo-2′,4′,5′-trimethoxystilbene was used instead of alpha-cyano-4-bromo-2′,4′,5′-trimethoxystilbene: STR133 melting point of the obtained compound was 273-276 C.

The synthetic route of 51628-12-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Morinaga Milk Industry Co., Ltd.; US5574062; (1996); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 103440-52-4, These common heterocyclic compound, 103440-52-4, name is Methyl 2-Iodo-5-methylbenzoate, 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.

Add 1.65 g (10 mmol) to a 250 mL round bottom flask.2-Amino-5-methylbenzoic acid methyl ester, 6.07 g (22 mmol)Methyl 2-iodo-5-methylbenzoate, 3.32 g (24 mmol) potassium carbonate,0.26 g (4 mmol) of activated copper powder and 100 mL of o-dichlorobenzene,Degas the reaction system and then protect it with argon.The mixture was heated to 180 C with stirring and the reaction was continued for 72 h. After the reaction is complete,The system was cooled to room temperature, suction filtered under reduced pressure and the residue was washed with dichloromethane.After the filtrate is dried,With dichloromethane:The petroleum ether = 4:1 (volume ratio) eluent was separated and purified on a silica gel column.Obtained a yellow solid 3.38g,The yield was 73.2%.

Statistics shows that Methyl 2-Iodo-5-methylbenzoate is playing an increasingly important role. we look forward to future research findings about 103440-52-4.

Reference:
Patent; Soochow University (Suzhou); Liao Liangsheng; Yuan Yi; Jiang Zuoquan; (46 pag.)CN109456326; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 199850-56-1, name is Methyl 2-amino-4-chloro-5-iodobenzoate, 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 199850-56-1, Recommanded Product: 199850-56-1

Intermediate 92 : Methyl 4-chloro-5-iodo-2-(2-(phenylsulfonyl)acetamido)benzoateTo a solution of 2-(phenylsulfonyl) acetic acid (Lancaster Synthesis Ltd., 0.771 mg, 3.85 mmol) in dichloromethane (50 mL) was added oxalyl chloride (4.17 mL, 4.17 mmol) and few drops of DMF. The reaction mixture was stirred 2 hours at room temperature. To a solution of methyl 2-amino-4-chloro-5-iodobenzoate (Intermediate 2) (1 g, 3.21 mmol) and triethylamine (1.074 mL, 7.70 mmol) in dichloromethane (50 mL) at RT was added dropwise the acid chloride prepared above. The reaction mixture was stirred at room temperature overnight then quenched with aqueous solution of NaHC03. The organic layer was and washed with saturated NaHC03, water and brine. The organic layer was dried over anhydrous Na2S04, filtered and concentrated in vacuo to give the title compound methyl 4- chloro-5-iodo-2-(2-(phenylsulfonyl)acetamido)benzoate (1.1 g, 2.228 mmol, 69.4 % yield) as pale yellow powder. LCMS: (M+H)+ = 494 ; Rt = 3.58 min.

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, Methyl 2-amino-4-chloro-5-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXOSMITHKLINE LLC; DAUGAN, Alain Claude-Marie; LAMOTTE, Yann; MIRGUET, Olivier; WO2012/119978; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com