Ammonia → HCID 20189398, 화합물

HRID 1789028노트

반응식

HRID 1789028 반응식
[F:1][CH2:2][C:3](=O)[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[N+:11]([C:14]1[CH:15]=[C:16]([CH:20]=[C:21]([C:27](=O)[CH3:28])[C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:17]=[CH:18][CH:19]=1)([O-:13])=[O:12].[NH3:30]>C(O)C>[F:1][CH2:2][C:3]1[NH:30][C:27]([CH3:28])=[C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH:20]([C:16]2[CH:17]=[CH:18][CH:19]=[C:14]([N+:11]([O-:13])=[O:12])[CH:15]=2)[C:4]=1[C:5]([O:7][CH2:8][CH3:9])=[O:6]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 9744Ethyl 4-fluoro-3-oxobutanoateHCID 367507Ethyl 2-(3-nitrobenzylidene)-3-oxobutanoate

생성물 1

HCID 20189398HCID 20189398, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl 4-fluoro-3-oxobutanoate (1.45 g, 10 mmoles), ethyl 2-(3-nitrophenylmethylene)-3-oxobutanoate (2.63 g, 10 mmoles) and aqueous ammonia (1.1 ml, d 0.88) were heated at reflux in ethanol (15 ml) for 6 hours. The solvent was removed in vacuo and the residue purified by chromatography on silica eluting with petroleum ether (60°-80° )/ether mixtures. Recrystallisation from ether/petroleum ether (60°-80° ) gave the title compound (1.1 g) as yellow crystals mp 139°-41°.

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residue purified by chromatography on silica eluting with petroleum ether (60°-80° )/ether mixtures
  3. customRecrystallisation from ether/petroleum ether (60°-80° )

출처 및 근거

ORD 기록
ord-a5355033654e4c89a95591098884e086
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04686217

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