Propane sultone → 3-({1-[1-(4-Chlorophenyl)cyclobutyl]-3,4-dihydroisoquinolin-7-yl}oxy)propane-1-sulfonic acid

HRID 242087ノート

反応式

HRID 242087 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:12]3[C:21]4[C:16](=[CH:17][CH:18]=[C:19]([OH:22])[CH:20]=4)[CH2:15][CH2:14][N:13]=3)[CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[H-].[Na+].[CH2:25]1[CH2:31][S:28](=[O:30])(=[O:29])[O:27][CH2:26]1>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([C:12]3[C:21]4[C:16](=[CH:17][CH:18]=[C:19]([O:22][CH2:26][CH2:25][CH2:31][S:28]([OH:30])(=[O:29])=[O:27])[CH:20]=4)[CH2:15][CH2:14][N:13]=3)[CH2:11][CH2:10][CH2:9]2)=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 14264Propane sultoneHCID 24758Sodium hydrideHCID 582462431-[1-(4-Chlorophenyl)cyclobutyl]-3,4-dihydroisoquinolin-7-ol

生成物 1

HCID 582463633-({1-[1-(4-Chlorophenyl)cyclobutyl]-3,4-dihydroisoquinolin-7-yl}oxy)propane-1-sulfonic acid

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The crude 1-[1-(4-chlorophenyl)cyclobutyl]-3,4-dihydroisoquinolin-7-ol (3.5 g, 11.22 mmol) was added to a suspension of sodium hydride (60% in mineral oil, 471 mg, 11.79 mmol) in dimethylformamide (25 mL). After stirring for 30 min at room temperature 1,3-propanesultone (1.44 g, 11.79 mmol) was added dropwise. The reaction mixture was stirred over night at room temperature. The dimethylformamide was removed in vacuo. The crude product (8.4 g) was used for the next step without further purification.

後処理

  1. additionwas added dropwise
  2. customThe dimethylformamide was removed in vacuo
  3. customThe crude product (8.4 g) was used for the next step without further purification

出典と根拠

ORDレコード
ord-d107030a440a4fcdaa364814be7bf77a
出典データセット
uspto-grants-2014_02
特許番号
US08653100B2

反応ノート

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