m-Chloroperbenzoic acid → 4-Acetyl-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide

HRID 1079323노트

반응식

HRID 1079323 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[C:12]([N:15]1[CH2:21][C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=2[S:18][CH2:17][CH2:16]1)(=[O:14])[CH3:13]>ClCCl>[C:12]([N:15]1[CH2:21][C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=2[S:18](=[O:9])[CH2:17][CH2:16]1)(=[O:14])[CH3:13]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 146707161-(2,3-Dihydro-1,4-benzothiazepin-4(5H)-yl)ethanone

생성물 1

HCID 233666804-Acetyl-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 3-chloroperbenzoic acid (1.03 g) in dichloromethane (100 ml) was added dropwise with cooling from 0° C. to -2° C. to a stirred solution of 4-acetyl-2,3,4,5-tetrahydro-1,4-benzothiazepine (1.03 g, prepared as Example 7 above) in dichloromethane (50 ml). The reaction mixture was stirred for 15 minutes, then washed with water, dried and the solvent was removed by evaporation at reduced pressure. Purification of the residue by flash chromatography using dichloromethane/ethanol (9:1) as eluent gave 4-acetyl-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide, which was recrystallised from ethyl acetate. Yield 0.67 g (m.p. 156°-157° C.).

후처리

  1. washwashed with water
  2. customdried
  3. customthe solvent was removed by evaporation at reduced pressure
  4. customPurification of the residue by flash chromatography

출처 및 근거

ORD 기록
ord-ac0ad43324354903b155ff0fc8ba8018
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580866

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