Hydrochloric Acid → 6-Chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine

HRID 1079331

반응식

HRID 1079331 반응식
[CH3:1][S:2](Cl)=[O:3].[Cl:5][C:6]1[C:11]2[CH2:12][NH:13][CH2:14][CH2:15][S:16][C:10]=2[CH:9]=[CH:8][CH:7]=1.Cl.C(N(CC)CC)C>ClCCl>[Cl:5][C:6]1[C:11]2[CH2:12][N:13]([S:2]([CH3:1])=[O:3])[CH2:14][CH2:15][S:16][C:10]=2[CH:9]=[CH:8][CH:7]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 548463Methanesulfinyl chlorideHCID 10198105HCID 10198105, 화합물

생성물 1

HCID 98816666-Chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of methanesulphinyl chloride (0.98 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/ethanol (98:2) as eluent gave 6-chloro-4-methylsulphinyl-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from ethylacetate/hexane. Yield 2.1 g (m.p. 82°-84° 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-a4b39ac55d1746fba3b43ffd23dfb566
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580866

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