m-Chloroperbenzoic acid → 6-Chloro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide

HRID 1079335노트

반응식

HRID 1079335 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[Cl:12][C:13]1[C:18]2[CH2:19][N:20]([S:24]([CH3:27])(=[O:26])=[O:25])[CH2:21][CH2:22][S:23][C:17]=2[CH:16]=[CH:15][CH:14]=1>ClCCl>[Cl:12][C:13]1[C:18]2[CH2:19][N:20]([S:24]([CH3:27])(=[O:26])=[O:25])[CH2:21][CH2:22][S:23](=[O:9])[C:17]=2[CH:16]=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 233666796-Chloro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine

생성물 1

HCID 233666876-Chloro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 3-chloroperbenzoic acid (2.26 g) in dichloromethane (150 ml) was added dropwise with cooling from 0° C. to -2° C. to a stirred solution of 6-chloro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine (3.05 g, prepared as Example 19 above) in dichloromethane (100 ml). The reaction mixture was stirred for 15 minutes, washed with water and dried, and the solvent was removed by evaporation at reduced pressure. Purification of the residue by flash chromatography using dichloromethane/ethanol (95:5) as eluent gave 6-chloro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide, which was recrystallised from ethyl acetate. Yield 2.86 g (m.p. 167°-169° 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-cd755516cb0f4766ae16648f7dbf74e3
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580866

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