Water → 4'-(4-Chloro-5-formyl-2-phenylimidazol-1-ylmethyl)biphenyl-2-sulfonic acid dimethylaminomethylenamide

HRID 1019246노트

반응식

HRID 1019246 반응식
[Cl:1][C:2]1[N:3]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[NH:5][C:6]=1[CH:7]=[O:8].[CH3:15][N:16]([CH:18]=[N:19][S:20]([C:23]1[C:24]([C:29]2[CH:34]=[CH:33][C:32]([CH2:35]Br)=[CH:31][CH:30]=2)=[CH:25][CH:26]=[CH:27][CH:28]=1)(=[O:22])=[O:21])[CH3:17].C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[CH3:17][N:16]([CH:18]=[N:19][S:20]([C:23]1[C:24]([C:29]2[CH:30]=[CH:31][C:32]([CH2:35][N:5]3[C:6]([CH:7]=[O:8])=[C:2]([Cl:1])[N:3]=[C:4]3[C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=3)=[CH:33][CH:34]=2)=[CH:25][CH:26]=[CH:27][CH:28]=1)(=[O:22])=[O:21])[CH3:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 541617064'-Bromomethylbiphenyl-2-sulfonic acid dimethylaminomethylenamideHCID 178520008HCID 178520008, 화합물

생성물 1

HCID 867577064'-(4-Chloro-5-formyl-2-phenylimidazol-1-ylmethyl)biphenyl-2-sulfonic acid dimethylaminomethylenamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2.1 g of 4-chloro-5-formyl-2-phenylimidazole (Chem. Pharm. Bull. 1976, 24(5), 960), 3.8 g of 4′-bromomethylbiphenyl-2-sulfonic acid dimethylaminomethylenamide (J. Med. Chem. 1995, 38, 2357) and 2.8 g of K2CO3 were stirred at RT for 30 h in 50 ml of DMF. The reaction mixture was poured onto 500 ml of water and extracted 2 times using 250 ml of EA each time. The organic phase was then washed with 100 ml of water and dried over MgSO4, and the solvent was removed in vacuo. Chromatography on silica gel using MTB yielded 1.9 g of a white, crystalline powder, mp 193° C.

후처리

  1. extractionextracted 2 times
  2. washThe organic phase was then washed with 100 ml of water
  3. dry with materialdried over MgSO4
  4. customthe solvent was removed in vacuo
  5. customChromatography on silica gel using MTB yielded 1.9 g of a white, crystalline powder, mp 193° C.

출처 및 근거

ORD 기록
ord-d1e9163aae7a4bea856f3572f93277bf
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06486189B2

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