Pyridine → 4-Diacetylamino-2-bromothiazole

HRID 26199노트

반응식

HRID 26199 반응식
[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]

참가 물질

4

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 202940434-Acetamido-2-bromo-thiazole

생성물 1

HCID 203771654-Diacetylamino-2-bromothiazole수율 10.7%

실험 절차

A solution of 4-acetylamino-2-bromothiazole 10 g, 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; N, 10.6 C7H7BrN2O2S requires C, 32.0; H, 2.7; N, 10.7%)

후처리

  1. temperatureThe reaction mixture was cooled
  2. customthe excess acetic anhydride and pyridine removed in vacuo
  3. customthe residue was re-evaporated three times with toluene
  4. customThe residue was purified by column chromatography
  5. washeluting with chloroform
  6. customrecrystallised from hexane

출처 및 근거

ORD 기록
ord-47f7e7441b0743cd9732fce06a051fe2
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04148904

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