Chlorosulfonic acid → 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonyl chloride

HRID 395270노트

반응식

HRID 395270 반응식
[C:1]([N:4]1[CH2:10][CH2:9][C:8]2[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=2[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Cl:15][S:16](O)(=[O:18])=[O:17]>ClCCl>[C:1]([N:4]1[CH2:10][CH2:9][C:8]2[CH:11]=[CH:12][C:13]([S:16]([Cl:15])(=[O:18])=[O:17])=[CH:14][C:7]=2[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 193754873-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine

생성물 1

HCID 113467373-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonyl chloride수율 45%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine (4.0 g, 0.021 mol) in dichloromethane (25 ml) was added dropwise to a stirred solution of chlorosulphonic acid in dichloromethane (25 ml) at −70° C. under argon. After warming to room temperature, the reaction was stirred for 18 h before being quenched in ice/water (200 ml). The resulting mixture was extracted with ethyl acetate (3×100 ml), dried (Na2SO4) and the solvent evaporated in vacuo to give the title compound (2.74 g, 45%) as a pale yellow solid.

후처리

  1. custombefore being quenched in ice/water (200 ml)
  2. extractionThe resulting mixture was extracted with ethyl acetate (3×100 ml)
  3. dry with materialdried (Na2SO4)
  4. customthe solvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-d683a4d4905d419a8b71d580055abd26
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06605607B1

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