Acetic Anhydride → 1-(2,3-Dihydro-1,4-benzothiazepin-4(5H)-yl)ethanone

HRID 1079322노트

반응식

HRID 1079322 반응식
[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][CH2:3][CH2:2]1.[C:12](OC(=O)C)(=[O:14])[CH3:13]>>[C:12]([N:4]1[CH2:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[S:1][CH2:2][CH2:3]1)(=[O:14])[CH3:13]

참가 물질

3

반응물 2

HCID 7918Acetic AnhydrideHCID 122691062,3,4,5-Tetrahydrobenzo[f][1,4]thiazepine

생성물 1

HCID 146707161-(2,3-Dihydro-1,4-benzothiazepin-4(5H)-yl)ethanone

실험 절차

A solution of 2,3,4,5-tetrahydro-1,4-benzothiazepine (1.5 g, prepared as described in the first paragraph of Example 6 above) in acetic anhydride (15 ml) was stirred at room temperature for one hour. The reaction mixture was poured into ice and extracted with dichloromethane. The organic layer was dried and the solvent removed by evaporation to give 4-acetyl-2,3,4,5-tetrahydro-1,4-benzothiazepine [a compound known as a Friedel Crafts catalyst from Example 46 of EP 368063 (Bayer)]. The product was recrystallised from hexane. Yield 1.55 g (m.p. 69°-70° C.).

후처리

  1. additionThe reaction mixture was poured into ice
  2. extractionextracted with dichloromethane
  3. customThe organic layer was dried
  4. customthe solvent removed by evaporation

출처 및 근거

ORD 기록
ord-b9f18c8655a4479299f893d01729096d
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580866

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