Pyridine → 4-Diacetylamino-2-bromothiazole
反応式
[C:1]([NH:4][C:5]1[N:6]=[C:7]([Br:10])[S:8][CH:9]=1)(=[O:3])[CH3:2].N1C=CC=CC=1.[C:17](OC(=O)C)(=[O:19])[CH3:18]>>[C:1]([N:4]([C:17](=[O:19])[CH3:18])[C:5]1[N:6]=[C:7]([Br:10])[S:8][CH:9]=1)(=[O:3])[CH3:2]参加物
4
実験手順
A solution of 4-acetylamino-2-bromothiazole 10g, prepared as described in Example 1, in acetic anhydride (100 ml) and pyridine (35 ml) was stirred at 100° C. for 24 hours. The reaction mixture was cooled and the excess acetic anhydride and pyridine removed in vacuo, and the residue was re-evaporated three times with toluene. The residue was purified by column chromatography using silica gel and eluting with chloroform, and recrystallised from hexane to give the title compound (1.2 g) m.p. 63°-65° C. (Found: C, 32.1; H, 2.8; H, 10.6 C7H7BrN2O2S requires C, 32.0; H, 2.7; N, 10.7%)
後処理
- temperatureThe reaction mixture was cooled
- customthe excess acetic anhydride and pyridine removed in vacuo
- customthe residue was re-evaporated three times with toluene
- customThe residue was purified by column chromatography
- washeluting with chloroform
- customrecrystallised from hexane
出典と根拠
- ORDレコード
- ord-4a82443f8bda4e489044999ff724092f
- 出典データセット
- uspto-grants-1980_01
- 特許番号
- US04183854
反応ノート
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