2-(n-Propoxy)ethyl 3-aminocrotonate → 2-n-Propoxyethyl 2,6-dimethyl-4-(3-nitrophenyl)-5-diisopropoxyphosphinyl-1,4-dihydropyridine-3-carboxylate

HRID 485075노트

반응식

HRID 485075 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:22]=[CH:23][CH:24]=1)[CH:7]=[C:8]([P:12](=[O:21])([O:17][CH:18]([CH3:20])[CH3:19])[O:13][CH:14]([CH3:16])[CH3:15])[C:9]([CH3:11])=O)([O-:3])=[O:2].[NH2:25]/[C:26](/[CH3:37])=[CH:27]\[C:28]([O:30][CH2:31][CH2:32][O:33][CH2:34][CH2:35][CH3:36])=[O:29]>C(O)(C)C>[CH3:37][C:26]1[NH:25][C:9]([CH3:11])=[C:8]([P:12]([O:17][CH:18]([CH3:20])[CH3:19])([O:13][CH:14]([CH3:16])[CH3:15])=[O:21])[CH:7]([C:6]2[CH:22]=[CH:23][CH:24]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[C:27]=1[C:28]([O:30][CH2:31][CH2:32][O:33][CH2:34][CH2:35][CH3:36])=[O:29]

참가 물질

4

반응물 2

HCID 125291902-(n-Propoxy)ethyl 3-aminocrotonateHCID 54197951Diisopropyl 1-(3-nitrobenzylidene)-acetonylphosphonate

생성물 1

HCID 133636722-n-Propoxyethyl 2,6-dimethyl-4-(3-nitrophenyl)-5-diisopropoxyphosphinyl-1,4-dihydropyridine-3-carboxylate수율 72%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 5.1 grams of diisopropyl 1-(3-nitrobenzylidene)-acetonylphosphonate and 2.69 grams of 2-n-propoxyethyl 3-aminocrotonate was added to 20 ml of isopropanol and the mixture was heated to reflux for eight hours with stirring. The reaction mixture was evaporated in vacuo, to the residue was added ether to crystallize, the crystals were collected by filtration, and recrystallized from a mixture of ethyl acetate and ether to afford 5.38 grams of 2-n-propoxyethyl 2,6-dimethyl-4-(3-nitrophenyl)-5-diisopropoxyphosphinyl-1,4-dihydropyridine-3-carboxylate, pale yellow crystals, melting point 125°-6° C. Yield 72%.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for eight hours
  3. customThe reaction mixture was evaporated in vacuo, to the residue
  4. additionwas added ether
  5. customto crystallize
  6. filtrationthe crystals were collected by filtration
  7. customrecrystallized from a mixture of ethyl acetate and ether

출처 및 근거

ORD 기록
ord-424b9c2d448a4e81b8df8e93230f9791
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04535073

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