6-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine → 6-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide

HRID 1079318ノート

反応式

HRID 1079318 の反応式
I([O-])(=O)(=O)=[O:2].[Na+].[Cl:7][C:8]1[C:13]2[CH2:14][NH:15][CH2:16][CH2:17][S:18][C:12]=2[CH:11]=[CH:10][CH:9]=1>O.ClCCl>[Cl:7][C:8]1[C:13]2[CH2:14][NH:15][CH2:16][CH2:17][S:18](=[O:2])[C:12]=2[CH:11]=[CH:10][CH:9]=1

参加物

5

反応物 2

HCID 101981056-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepineHCID 23667635Sodium periodate

生成物 1

HCID 101982836-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of sodium periodate (3.09 g) in water (25 ml) was added dropwise with cooling to a stirred solution of 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine (2.88 g, prepared in a similar manner to that described in the preceding paragraph) in dichloromethane (75 ml). The stirring was continued at room temperature for 19 hours. Solvent was removed from the mixture by evaporation at reduced pressure. Purification of the residue by flash chromatography using dichloromethane/ethanol (95:5) as eluent gave 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine 1-oxide, which was recrystallised from ethyl acetate. Yield 2.15 g (m.p. 125°-126° C.).

後処理

  1. customprepared in a similar manner to that
  2. customSolvent was removed from the mixture by evaporation at reduced pressure
  3. customPurification of the residue by flash chromatography

出典と根拠

ORDレコード
ord-e461df2775b74cb6841dc801026e2459
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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