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Ethanol → HCID 70874350, 화합물

HRID 1526124
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HRID 1526124 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 70874350HCID 70874350, 화합물수율 99.9%

시약·촉매·용매 1

HCID 8471
Triethylamine
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0254ffdc0c21408d97feb98cf167ac4f
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09085575B2

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