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

HRID 1079339노트

반응식

HRID 1079339 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.).

후처리

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

출처 및 근거

ORD 기록
ord-83413fc529ae43c3a14d0629d49d9166
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580866

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