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

HRID 1079322ノート

反応式

HRID 1079322 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.).

後処理

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

出典と根拠

ORDレコード
ord-b9f18c8655a4479299f893d01729096d
出典データセット
uspto-grants-1996_12
特許番号
US05580866

反応ノート

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