Month: August 2021

Related Products of 76801-93-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(b) (+)-5-Acetamido-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-isophthalamide The dextrorotatory compound was prepared from (+)-5-amino-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-isophthalamide (21 g) by acetylation and a subsequent hydrolysis at pH 10-11 in a similar manner to that described in C(a) above. Finally the product was recrystallized from water. Yield: 13.6 g (61%) [alpha]546 =+4.0; [alpha]578 =+3.8 (c=4.5; DMF:H2 O=2:8). Melting Point: 285-289 dec. Analysis–Found: C, 25.80; H, 2.50; I, 50.6; N, 5.71. Calc. for C16 H20 I3 N3 O7: C, 25.72; H, 2.70; I, 50.95; N, 5.62.

The synthetic route of 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nyegaard & Co. A/S; US4250113; (1981); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 19821-80-8, name is 1,3-Dibromo-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 19821-80-8

Synthesis Example 2 (Synthesis of 2,6-Dimesityliodobenzene) A solvent of 200 mL of THF was added to 6.0 g (250 mmol) of magnesium (Wako Pure Chemical Industries, Ltd.) and a trace amount of iodine. In 100 mL of THF was dissolved 34 mL (225 mmol) of bromomesitylene (Wako Pure Chemical Industries, Ltd.). The solution was added dropwise to the above magnesium/THF slurry at room temperature in 2 hours. After the completion of the dropping, the solution was refluxed for 2 hours, and then cooled to room temperature. In 50 mL of THF was dissolved 23 g (64 mmol) of 1,3-dibromoiodobenzene. The solution was added dropwise to the above Grignard solution at room temperature in 1 hour. The reaction liquid was refluxed for 3 hours, and then cooled to 0C. A solution of 25 g (100 mmol) of iodine in 50 mL of THF was added dropwise to the reaction mixture, followed by warming to room temperature. The reaction mixture was washed with a saturated aqueous solution of sodium sulfite, and then extracted three times with diethyl ether. The ether layers were mixed, then washed with water and saturated brine, and then dried with magnesium sulfate. The solvent was removed under reduced pressure, and the byproduct was then removed under reduced pressure. The residue was recrystallized from methanol, giving 19.7 g of white solid of 2,6-dimesityliodobenzene (70% in yield). It was confirmed that the product was 2,6-dimesityliodobenzene by 1H-NMR. 1H-NMR (400MHz, CDCl3) 1.98 (s, 12H, o-CH3), 2.35 (s, 6H, p-CH3), 6.96 [s, 4H, m-H (Mes)], 7.08 [d, J = 7.6 Hz, 2H, m-H (Ph)], 7.46 [t, J = 7.6 Hz, 1H, p-H (Ph)].

The synthetic route of 19821-80-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Otsuka Chemical Holdings Co., Ltd.; EP2133357; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic 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. Quality Control of 2-Iodo-4,5-dimethoxybenzoic acid

General procedure: DMF (2 drops) and oxalyl chloride (180 muL, 2.12 mmol) were added to a suspension of 4-chloro-2-iodobenzoic acid (0.400 g, 1.42mmol) in toluene (5 mL). After the acid had dissolved and evolution of gas had ceased, the mixture was concentrated under vacuum to afford the crude acyl chloride, which was used without further purification.To a soln of this crude acyl chloride in CH2Cl2 (6 mL) was added a soln of Et3N (592 muL, 4.25 mmol) and aniline (129 muL,1.42 mmol) in CH2Cl2 (6 mL). The mixture was stirred for 1 h and then sat. aq NH4Cl soln (5 mL) was added. The aq layer was extracted with CH2Cl2 (3 × 5 mL) and the combined organic layers dried (Na2SO4) and evaporated. The crude residue was purified by flash chromatography (hexanes-EtOAc, 90:10 to 85:15), to afford 5e (400 mg, 79%) as a white solid.

The synthetic route of 61203-48-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Madich, Youssef; Denis, J.Gabriel; Ortega, Aitor; Martinez, Claudio; Matrane, Abdellatif; Belachemi, Larbi; De Lera, Angel R.; Alvarez, Rosana; Aurrecoechea, Jose M.; Synthesis; vol. 45; 14; (2013); p. 2009 – 2017;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C6H3Cl2I

In a solution of 5.0 g of 3,5-dichloro-1-iodobenzene in 50 ml of t-butylmethylether, 12.2 ml of n-butyl lithium (1.58M hexane solution) was added dropwise at -78°C with stirring, after the completion of the addtion dropwise, stirred at the same temperature for 30 minutes. 6.6 g of chlorodifluoroacetic acid methyl ester was added dropwise at -78°C with stirring in the reaction mixture, after the completion of the addition drropwise, continued to stir at 0°C for further 30 minutes. After the completion of the reaction, the reaction mixture was poured in 100 ml of saturated ammonium chloride aqueous solution, extracted with ethyl acetate (100 ml x 1). The organic phase was dehydrated with saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure to obtain 4.6 g of crude aimed product as pale yellow oily substance. The resulting product was used as such without purification for the next step. 1H NMR (CDCl3, Me4Si, 300MHz) delta7.97 (s, 2H), 7.68 (s, 1 H).

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nissan Chemical Industries, Ltd.; EP1731512; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 40400-15-5, The chemical industry reduces the impact on the environment during synthesis 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, I believe this compound will play a more active role in future production and life.

isatin(1.0 mmol) was added to a 50 mL dry round bottom flask in turn.O-iodophenylacetonitrile (1.0 mmol), 4-hydroxycoumarin (1.0 mmol),Catalyst 3e (5 mol%), palladium dichloride (5 mol%),KOH (20 mol%), DMSO 3 mL, mix well, stir at 110 C,After the reaction was completed (TLC tracking), an appropriate amount of water was added and extracted with ethyl acetate.The organic phases are combined, and the excess solvent in the system is distilled off under reduced pressure.The crude product was separated by column chromatography (V petroleum ether: V ethyl acetate = 1:1 gradient elution) to give the title compound 12a in a yield of 88%

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-(2-Iodophenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Jiangsu Normal University; Chen Wen; Yuan Rui; Cui Hao; Ren Xuanxuan; Zhou Shengliang; Wan Yu; Wu Hui; (19 pag.)CN109305970; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 28547-29-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 28547-29-7, name is 2-Bromo-4-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 6 Preparation of ethyl 2-bromo-4-iodobenzoate (C60) To a stirred solution of 4-iodo-2-bromobenzoic acid (5.00 g, 15.3 mmol) in ethyl alcohol (100 mL) was added sulfuric acid (5 mL), and the reaction mixture was heated at 80 C. for 18 hours. The reaction mixture was cooled to 25 C. and concentrated under reduced pressure. The residue was diluted with ethyl acetate (2*100 mL) and washed with water (100 mL). The combined ethyl acetate extracts were washed with brine, dried over sodium sulfate, and concentrated under reduced pressure to afford the compound as a pale yellow solid (5.00 g, 92%): 1H NMR (400 MHz, DMSO-d6) delta 8.04 (d, J=1.2 Hz, 1H), 7.71 (d, J=7.6 Hz, 1H), 7.51 (d, J=8.4 Hz, 1H), 4.41 (q, J=7.2 Hz, 2H), 1.41 (t, J=7.2 Hz, 3H).

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-Bromo-4-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DOW AGROSCIENCES LLC; LePlae, JR., Paul Renee; Hunter, James E.; Watson, Gerald B.; Lo, William C.; Herbert, John; US2015/353477; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 20776-54-9, name is 2-Amino-4-iodobenzoic acid, 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. Product Details of 20776-54-9

Embodiment 22 2-amino-4-((4,4-dimethyl-1-oxothiochroman-6-yl)ethynyl)benzoic acid 1-oxo-6-ethynyl-4,4-dimethylbenzothiopyran (263mg, 1.0mmol) and 2-amino-4-iodobenzoic acid (262mg, 1.2mmol) were added to a flask, followed by addition of Pd(PPh3)2Cl2 (42mg, 0.06mmol) and CuI (23mg, 0.0412mmol). After the flask was purged with argon for 3 times to remove oxygen, 4mL dry DMF and 0.2mL dry Et3N were added via syringe. Then the reaction was continued at 70C for 8 h and monitored by TLC. After completion of the reaction, the reaction solution was cooled to room temperature and the reaction was quenched with saturated ammonium chloride solution. The mixture was diluted with ethyl acetate, washed with saturated ammonium chloride solution and saturated sodium chloride solution. The organic phase was dried over anhydrous sodium sulfate, filtered, concentrated and purified by flash column chromatography (PE:EtOAc = 50:1) to give the product (275 mg, 78%). 1H NMR (500 MHz, pyridine) delta 8.37 (d, J = 8.1 Hz, 1H), 7.92 (d, J = 8.0 Hz, 1H), 7.86 (s, 1H), 7.59 (s, 1H), 7.36 (s, 1H), 7.03 (d, J = 8.1 Hz, 1H), 5.67 (s, 1H), 3.20 – 3.14 (m, 1H), 3.11 – 3.05 (m, 1H), 2.38 (ddd, J = 14.2, 10.3, 1.7 Hz, 1H), 1.74 – 1.68 (m, 1H), 1.26 (s, 3H), 1.17 (s, 3H); 13C NMR (126 MHz, pyridine) delta 171.06, 152.34, 145.52, 140.46, 132.80, 131.65, 130.43, 130.20, 127.92, 126.32, 119.79, 118.58, 112.43, 91.82, 90.33, 55.01, 43.59, 34.63, 30.93, 30.63, 29.80. ESI(+)-MS: 354.3 [M+1]+.

The synthetic route of 2-Amino-4-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences; Huazhong University of Science and Technology; CAO, Xin; YU, Biao; WANG, Ning; CHEN, Junwei; (88 pag.)EP3428155; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, molecular formula is C6H3BrINO2, 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. Computed Properties of C6H3BrINO2

(1) Take (100mmol) 4- (9,9-dimethylphosphonium) boronic acid,32.6g (100mmol) of 2-iodo-5-bromonitrobenzene,(1%) Pd (PPh3) 4,40g (300mmol) sodium carbonate,Toluene (800mL),Ethanol (200 mL) and water (200 mL),Heated to reflux, reacted for 8h, the reaction was completed;The reaction solution was extracted with ethyl acetate, and the organic phase was concentrated.A yellow solid A was obtained;

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 112671-42-8, its application will become more common.

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (28 pag.)CN110698458; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 27913-58-2,Some common heterocyclic compound, 27913-58-2, name is 4-(4-Iodophenyl)butanoic acid, molecular formula is C10H11IO2, 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.

(g) 74-p-iodophenyl-butric acid (502 mg, 1.7 mmol, 1.07 eq. ) was dissolved in DMF (1.5 ml) and NEt3 (2 eq.). HBTU (751 mg, 1.98 mmol, 1.23 eq.) was added. The solution was stirred at 0 C for 1 h. The solution was added drop wise to Boc-Lys-OMe (428 mg, 1.6 ramol) in DMF (1.5 ml) and Et3 (2 eq.). The solution was stirred at 0 C for 4 h. The product was extracted with citric acid (1 M) and ethyl acetate/n-Hexane (9:1). The organic phase was rinsed with brine, dried over a2S04 and concentrated under reduced pressure. Purification was achieved by CC (SiC>2,MeOH/CH2Cl2 1:50) to give a clear oil. 653.5 mg (1.23 mmol, 75%). LC-MS [M+H]+ = 532.77 (calc. for C22H33IN2O5, 532.14). 1H-NMR (MeOH-d4) delta 7.59, 6.98, 4.09, 3.69, 3.15, 2.59, 2.29, 2.18, 1.88, 1.78/1.64, 1.51, 1.42 ppm

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-(4-Iodophenyl)butanoic acid, its application will become more common.

Reference:
Patent; MERCK & CIE; SCHIBLI, Roger; MOSER, Rudolf; MUeLLER, Cristina Magdalena; STRUTHERS, Harriet; GROEHN, Viola; AMETAMEY, Simon Mensah; FISCHER, Cindy Ramona; WO2013/24035; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 696-41-3, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 696-41-3, name is 3-Iodobenzaldehyde belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of 3-iodobenzaldehyde (200 mg, 0.862 mmol) in dry CH2Cl2 (10 mL)was added pyrrolidine (61.3 mg, 0.862 mmol). After 10 mins, sodium triacetoxyborohydride (190 mg, 0.90 mmol) was added and the reaction mixture was stirred at room temperature for1 h, then it was washed with saturated sodium bicarbonate solution, dried, and concentratedin vacuo. The crude was filtered through an isolute SCX-2 cartridge to give the titlecompound (205 mg, 83%);

The synthetic route of 3-Iodobenzaldehyde has been constantly updated, and we look forward to future research findings.

Reference:
Article; Le Bihan, Yann-Vai; Lanigan, Rachel M.; Atrash, Butrus; McLaughlin, Mark G.; Velupillai, Srikannathasan; Malcolm, Andrew G.; England, Katherine S.; Ruda, Gian Filippo; Mok, N. Yi; Tumber, Anthony; Tomlin, Kathy; Saville, Harry; Shehu, Erald; McAndrew, Craig; Carmichael, LeAnne; Bennett, James M.; Jeganathan, Fiona; Eve, Paul; Donovan, Adam; Hayes, Angela; Wood, Francesca; Raynaud, Florence I.; Fedorov, Oleg; Brennan, Paul E.; Burke, Rosemary; van Montfort, Rob L.M.; Rossanese, Olivia W.; Blagg, Julian; Bavetsias, Vassilios; European Journal of Medicinal Chemistry; vol. 177; (2019); p. 316 – 337;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com