Water → 4-[(3-Bromophenyl)amino]-6-[(4-{N-[(tert-butyloxycarbonyl)methyl]-N-[2-(acetylsulphanyl)ethyl]amino)-1-oxo-2-buten-1-yl)-amino]-7-methoxy-quinazoline

HRID 488421

반응식

HRID 488421 반응식
[C:1]([O-:4])(=[S:3])[CH3:2].[K+].[Br:6][C:7]1[CH:8]=[C:9]([NH:13][C:14]2[C:23]3[C:18](=[CH:19][C:20]([O:46][CH3:47])=[C:21]([NH:24][C:25](=[O:45])[CH:26]=[CH:27][CH2:28][N:29]([CH2:37][C:38]([O:40][C:41]([CH3:44])([CH3:43])[CH3:42])=[O:39])[CH2:30][CH2:31]OS(C)(=O)=O)[CH:22]=3)[N:17]=[CH:16][N:15]=2)[CH:10]=[CH:11][CH:12]=1.O>CN(C)C=O>[Br:6][C:7]1[CH:8]=[C:9]([NH:13][C:14]2[C:23]3[C:18](=[CH:19][C:20]([O:46][CH3:47])=[C:21]([NH:24][C:25](=[O:45])[CH:26]=[CH:27][CH2:28][N:29]([CH2:37][C:38]([O:40][C:41]([CH3:42])([CH3:44])[CH3:43])=[O:39])[CH2:30][CH2:31][S:3][C:1](=[O:4])[CH3:2])[CH:22]=3)[N:17]=[CH:16][N:15]=2)[CH:10]=[CH:11][CH:12]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 23670855Potassium ethanethioateHCID 572144434-[(3-bromophenyl)amino]-6-[(4-(N-[(tert-butyloxycarbonyl)methyl]-N-[2-(methylsulphonyloxy)ethyl]amino}-1-oxo-2-buten-1-yl)amino]-7-methoxy-quinazoline

생성물 1

HCID 738794514-[(3-Bromophenyl)amino]-6-[(4-{N-[(tert-butyloxycarbonyl)methyl]-N-[2-(acetylsulphanyl)ethyl]amino)-1-oxo-2-buten-1-yl)-amino]-7-methoxy-quinazoline

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

34 mg of potassium thioacetate are added to 150 mg of 4-[(3-bromophenyl)amino]-6-[(4-(N-[(tert-butyloxycarbonyl)methyl]-N-[2-(methylsulphonyloxy)ethyl]amino}-1-oxo-2-buten-1-yl)amino]-7-methoxy-quinazoline in 1 ml of dimethylformamide at ambient temperature. The reaction mixture is stirred overnight at ambient temperature and then combined with water for working up. The aqueous phase is separated off and extracted with ethyl acetate, the combined organic phases are dried over magnesium sulphate and freed from solvent in the rotary evaporator. Yield: 20 mg (14% of theory), Rf value: 0.62 (silica gel, ethyl acetate/methanol=15:1) Mass spectrum (EI): m/z=643, 645 [M]+

후처리

  1. customThe aqueous phase is separated off
  2. extractionextracted with ethyl acetate
  3. dry with materialthe combined organic phases are dried over magnesium sulphate
  4. customfreed from solvent in the rotary evaporator

출처 및 근거

ORD 기록
ord-96fe93f0c8294e8a818701511fb4c946
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06972288B1

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