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ノート

反応式

HRID 488421 の反応式
[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

参加物

5

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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]+

後処理

  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

出典と根拠

ORDレコード
ord-96fe93f0c8294e8a818701511fb4c946
出典データセット
uspto-grants-2005_12
特許番号
US06972288B1

反応ノート

読み込み中…