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

HRID 1079335ノート

反応式

HRID 1079335 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 233666876-Chloro-4-methylsulphonyl-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 (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.).

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-cd755516cb0f4766ae16648f7dbf74e3
出典データセット
uspto-grants-1996_12
特許番号
US05580866

反応ノート

読み込み中…