3-Chloropropanesulphonyl chloride → HCID 63362723, 화합물

HRID 408593

반응식

HRID 408593 반응식
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]

참가 물질

4

반응물 2

HCID 154103-Chloropropanesulphonyl chlorideHCID 30843432,4-Dimethoxybenzylamine hydrochloride

생성물 1

HCID 63362723HCID 63362723, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

반응 조건

온도
20 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e4ec7a6c826a4b9f8a59e6093972de0c
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759334B2

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