3-Chloropropanesulphonyl chloride → HCID 63362723、化合物

HRID 408593

反応式

HRID 408593 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:5]=1[CH2:6][NH2:7].[Cl:14][CH2:15][CH2:16][CH2:17][S:18](Cl)(=[O:20])=[O:19]>C(Cl)Cl>[CH3:2][O:3][C:4]1[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:5]=1[CH2:6][NH:7][S:18]([CH2:17][CH2:16][CH2:15][Cl:14])(=[O:20])=[O:19]

参加物

4

反応物 2

HCID 154103-Chloropropanesulphonyl chlorideHCID 30843432,4-Dimethoxybenzylamine hydrochloride

生成物 1

HCID 63362723HCID 63362723、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
20 °C

実験手順

To a solution of 2,4-dimethoxy-benzylamine hydrochloride (1 eq.) and TEA (2 eq.) in DCM was added dropwise at 0° C. a solution of 3-chloro-propane-1-sulfonyl chloride (1 eq.) in DCM. The reaction was stirred at 20° C. for 20 h. The crude was diluted with DCM, washed twice with water, twice with aqueous HCl (0.1N) and twice with a saturated aqueous solution of NaHCO3. The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. The crude was purified by chromatography on silica gel (elution with heptane/EtOAc: 100/0 to 20/80) to afford 3-chloro-propane-1-sulfonic acid 2,4-dimethoxy-benzylamide.

後処理

  1. washwashed twice with water, twice with aqueous HCl (0.1N) and twice with a saturated aqueous solution of NaHCO3
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude was purified by chromatography on silica gel (elution with heptane/EtOAc: 100/0 to 20/80)

出典と根拠

ORDレコード
ord-e4ec7a6c826a4b9f8a59e6093972de0c
出典データセット
uspto-grants-2014_06
特許番号
US08759334B2

関連ノート

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