Acetic Anhydride → Ethyl 6-fluoro-7-(pyrrol-1-yl)-1-formylamino-4-oxo-1,4-dihydroquinoline-3-carboxylate

HRID 4566

반응식

HRID 4566 반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N:12]1[CH:16]=[CH:15][CH:14]=[CH:13]1)[N:8]([NH2:17])[CH:7]=[C:6]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:5]2=[O:23].[C:24](OC(=O)C)(=[O:26])C>C(O)=O>[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N:12]1[CH:13]=[CH:14][CH:15]=[CH:16]1)[N:8]([NH:17][CH:24]=[O:26])[CH:7]=[C:6]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:5]2=[O:23]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 13670072Ethyl 6-fluoro-7-(pyrrol-1-yl)-1-amino-4-oxo-1,4-dihydroquinoline-3-carboxylate

생성물 1

HCID 13670073Ethyl 6-fluoro-7-(pyrrol-1-yl)-1-formylamino-4-oxo-1,4-dihydroquinoline-3-carboxylate

시약·촉매·용매 1

HCID 284Formic Acid용매2회

반응 조건

온도
0 °C

실험 절차

A solution of 3.15 g (0.01 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-1-amino-4-oxo-1,4-dihydroquinoline-3-carboxylate in 25 ml of formic acid is added dropwise to a mixture of 9.5 ml (0.01 mol) of acetic anhydride and 4 ml (0.01 mol) of formic acid, cooled to 0° C., the addition being carried out so as to maintain room temperature ±5° C. The mixture is kept at room temperature for48 hours and poured into a water/ice mixture, and the precipitate formed is filtered off, washed with water and recrystallized from a dimethylformamide/water mixture (1:1) to give a solid melting at 254°-257° C.

후처리

  1. additionthe addition
  2. temperatureto maintain room temperature ±5° C
  3. waitThe mixture is kept at room temperature for48 hours
  4. customthe precipitate formed
  5. filtrationis filtered off
  6. washwashed with water
  7. customrecrystallized from a dimethylformamide/water mixture (1:1)

출처 및 근거

ORD 기록
ord-8adc3019916d41df93e9978debdaa4cb
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727080

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