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Ethanol → HCID 70874350、化合物

HRID 1526124
ノート
印刷プレビュー

反応式

HRID 1526124 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:5][CH:4]=1.C(O)C.N1C=CC=CC=1.[C:26]([C:28](=[CH:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=1[N+:39]([O-:41])=[O:40])[C:29](=[S:31])[NH2:30])#[N:27]>C(N(CC)CC)C>[C:26]([C:28]1[C:29](=[S:31])[NH:30][C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:32]=1[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=1[N+:39]([O-:41])=[O:40])#[N:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702EthanolHCID 1049PyridineHCID 76150Benzenepropanoic acid, 4-methoxy-beta-oxo-, ethyl esterHCID 28911832-Propenethioamide, 2-cyano-3-(2-nitrophenyl)-

生成物 1

HCID 70874350HCID 70874350、化合物収率 99.9%

試薬・触媒・溶媒 1

HCID 8471
Triethylamine
溶媒

実験手順

2.22 g (10 mmol) of ethyl 3-(4-methoxyphenyl)-3-oxopropanoate, 50 ml of ethanol, 5 ml of pyridine and 0.5 ml of triethylamine are added respectively to 2.33 g (10 mmol) of 2-cyano-3-(2-nitrophenyl)prop-2-enethioamide. The reaction mixture is stirred at reflux for 5 hours. After returning to room temperature, the solvent is evaporated and the reaction mixture is poured over crushed ice. Acetic acid is added until an acidic pH (2 to 3) is obtained. The precipitate formed is filtered, rinsed with water and diethyl ether, and then dried under vacuum to yield 4.35 g (92%) of ethyl 5-cyano-2-(4-methoxyphenyl)-4-(2-nitrophenyl)-6-thioxo-1,6-dihydropyridine-3-carboxylate in the form of a yellow powder.

後処理

  1. temperatureat reflux for 5 hours
  2. customAfter returning to room temperature
  3. customthe solvent is evaporated
  4. additionthe reaction mixture is poured
  5. customover crushed ice
  6. additionAcetic acid is added until an acidic pH (2 to 3)
  7. customis obtained
  8. customThe precipitate formed
  9. filtrationis filtered
  10. washrinsed with water and diethyl ether
  11. customdried under vacuum

出典と根拠

ORDレコード
ord-0254ffdc0c21408d97feb98cf167ac4f
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09085575B2

反応ノート

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