Ammonia → Diethyl 1,2,3,4-tetrahydro-2-hydroxy-6-methyl-4-(3-nitrophenyl)-2-(4-nitrophenyl)-3,5-pyridinedicarboxylate

HRID 364961노트

반응식

HRID 364961 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:17])[CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:6][CH:5]=1)([O-:3])=[O:2].[N+:18]([C:21]1[CH:22]=[C:23]([CH:27]=[C:28]([C:34](=O)[CH3:35])[C:29]([O:31][CH2:32][CH3:33])=[O:30])[CH:24]=[CH:25][CH:26]=1)([O-:20])=[O:19].[NH3:37]>C(O)C>[OH:17][C:10]1([C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)[CH:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:27]([C:23]2[CH:24]=[CH:25][CH:26]=[C:21]([N+:18]([O-:20])=[O:19])[CH:22]=2)[C:28]([C:29]([O:31][CH2:32][CH3:33])=[O:30])=[C:34]([CH3:35])[NH:37]1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 13281Benzenepropanoic acid, 4-nitro-beta-oxo-, ethyl esterHCID 367507Ethyl 2-(3-nitrobenzylidene)-3-oxobutanoate

생성물 1

HCID 20189315Diethyl 1,2,3,4-tetrahydro-2-hydroxy-6-methyl-4-(3-nitrophenyl)-2-(4-nitrophenyl)-3,5-pyridinedicarboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl 4-nitro-beta-oxobenzenepropanoate (4.74 g, 20 mmoles), ethyl 2-(3-nitrophenylmethylene)-3-oxobutanoate (5.26 g, 20 mmoles) and aqueous ammonia (2.2 ml, d0.88) were heated at reflux in ethanol (50 ml) for 1.5 hours. After cooling the product was filtered off and recrystallised from ethanol to give the title compound (2.6 g) mp 196°-7°.

후처리

  1. temperatureAfter cooling the product
  2. filtrationwas filtered off
  3. customrecrystallised from ethanol

출처 및 근거

ORD 기록
ord-3889b65d28b24086abd18ac50b41a51c
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04607041

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