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

HRID 485075ノート

反応式

HRID 485075 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-424b9c2d448a4e81b8df8e93230f9791
出典データセット
uspto-grants-1985_08
特許番号
US04535073

反応ノート

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