Hydrochloric Acid → 4-Ethylsulphonyl-6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine

HRID 1079339ノート

反応式

HRID 1079339 の反応式
[CH2:1]([S:3](Cl)(=[O:5])=[O:4])[CH3:2].[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.Cl.C(N(CC)CC)C>ClCCl>[CH2:1]([S:3]([N:15]1[CH2:14][C:13]2[C:8]([Cl:7])=[CH:9][CH:10]=[CH:11][C:12]=2[S:18][CH2:17][CH2:16]1)(=[O:5])=[O:4])[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 11667Ethanesulfonyl chlorideHCID 101981056-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine

生成物 1

HCID 233666774-Ethylsulphonyl-6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of ethanesulphonyl chloride (1.28 g) in dichloromethane (10 ml) was added dropwise at room temperature to a stirred solution of 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine (1.99 g, prepared in a similar manner to its hydrochloride, Example 1 above) and triethylamine (1.01 g) in dichloromethane (50 ml). The reaction mixture was stirred at room temperature for one hour, washed with water, dried and the solvent was removed by evaporation. Purification of the residue by flash chromatography using dichloromethane as eluent gave 4-ethylsulphonyl-6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from ethyl acetate/hexane. Yield 2.53 g (m.p. 126°-128° C.).

後処理

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

出典と根拠

ORDレコード
ord-83413fc529ae43c3a14d0629d49d9166
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…