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Water → HCID 57966444, 화합물

HRID 420586
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HRID 420586 반응식
[Cl:1][C:2]1[CH:28]=[CH:27][C:5]2[N:6]=[C:7]([N:9]3[CH2:13][CH2:12][CH:11]([NH:14][S:15]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[N+:24]([O-:26])=[O:25])(=[O:17])=[O:16])[CH2:10]3)[S:8][C:4]=2[CH:3]=1.[H-].[Na+].[CH3:31][O:32][C:33](=[O:43])[CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[C:37]([CH2:41]Br)[CH:36]=1.O>CN(C)C=O>[CH3:31][O:32][C:33](=[O:43])[CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[C:37]([CH2:41][N:14]([CH:11]2[CH2:12][CH2:13][N:9]([C:7]3[S:8][C:4]4[CH:3]=[C:2]([Cl:1])[CH:28]=[CH:27][C:5]=4[N:6]=3)[CH2:10]2)[S:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[N+:24]([O-:26])=[O:25])(=[O:16])=[O:17])[CH:36]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 10014651(3-Bromomethyl-phenyl)-acetic acid methyl esterHCID 57966935HCID 57966935, 화합물

생성물 1

HCID 57966444HCID 57966444, 화합물수율 60.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

N-[1(6-chlorobenzothiazole-2-yl)pyrrolidine-3-yl]-2-nitrobenzenesulfonamide (500 mg) was dissolved in dimethylformamide (5 mL). Sodium hydride (60%, oil, 50 mg) was added thereto and the mixture was stirred at room temperature for 1 hour. (3-bromomethylphenyl)acetic acid methyl ester (305 mg) was added thereto and the mixture was stirred for 16 hours. To the reaction solution was added water and extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over magnesium sulphate. The solvent was evaporated under reduced pressure and the residue was purified by column chromatograph on silica gel to give the title compound (412 mg). Yield: 60%.

후처리

  1. stirringthe mixture was stirred for 16 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over magnesium sulphate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by column chromatograph on silica gel

출처 및 근거

ORD 기록
ord-846e199b5d25488f83e06776297ec060
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08097610B2

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