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

HRID 1079323ノート

反応式

HRID 1079323 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.).

後処理

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

出典と根拠

ORDレコード
ord-ac0ad43324354903b155ff0fc8ba8018
出典データセット
uspto-grants-1996_12
特許番号
US05580866

反応ノート

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