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

HRID 1079334노트

반응식

HRID 1079334 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[Cl:6][C:7]1[C:12]2[CH2:13][NH:14][CH2:15][CH2:16][S:17][C:11]=2[CH:10]=[CH:9][CH:8]=1.Cl.C(N(CC)CC)C>ClCCl>[Cl:6][C:7]1[C:12]2[CH2:13][N:14]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:15][CH2:16][S:17][C:11]=2[CH:10]=[CH:9][CH:8]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 101981056-Chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine

생성물 1

HCID 233666796-Chloro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of methanesulphonyl chloride (3.43 g) in dichloromethane (30 ml) was added dropwise at room temperature to a stirred solution of 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine (5.2 g, prepared in a similar manner to its hydrochloride, Example 1 above) and triethylamine (3.03 g, 0.03 ml) in dichloromethane (100 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 6-chloro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from hexane. Yield 6.06 g (m.p. 85°-86° 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-67ce8a5006504e008e0d8f09b88363a1
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580866

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