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Selenium Dioxide → HCID 14010755, 화합물

HRID 255673
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HRID 255673 반응식
[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:20]([CH3:21])=[CH:19][C:18](=[O:22])[C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12]2)=[C:7]([CH3:23])[CH:6]=1)(=[O:3])[CH3:2].[Se](=O)=[O:25]>O1CCOCC1>[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:20]([CH:21]=[O:25])=[CH:19][C:18](=[O:22])[C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12]2)=[C:7]([CH3:23])[CH:6]=1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24007Selenium DioxideHCID 20183847HCID 20183847, 화합물

생성물 1

HCID 14010755HCID 14010755, 화합물수율 72%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

In 315 ml of dioxane was dissolved 10.5 g of methyl 1-(4-acetoxy-2-methylphenyl)-6-methyl-4-oxo-1,4-dihydronicotinate under heating, and 4.43 g of selenium dioxide was added thereto. They were reacted at 100° C. for 2 hours. After cooling the reaction mixture, to room temperature, selenium was removed by filtration, and then the solvent was removed by distillation under reduced pressure. The residue was purified by a column chromatography (Wako Silica Gel C-200; eluent: chloroform/ethanol (25:1 by volume) mixture) to obtain 7.9 g of methyl 1-(4-acetoxy-2-methylphenyl)-6-formyl-4-oxo-1,4-dihydronicotinate having a melting point of 216°-217° C.

후처리

  1. temperatureunder heating
  2. customThey were reacted at 100° C. for 2 hours
  3. temperatureAfter cooling the reaction mixture
  4. customto room temperature, selenium was removed by filtration
  5. customthe solvent was removed by distillation under reduced pressure
  6. customThe residue was purified by a column chromatography (Wako Silica Gel C-200; eluent: chloroform/ethanol (25:1 by volume) mixture)

출처 및 근거

ORD 기록
ord-015069a57ef44dec9c5f90e1b7788f77
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04698352

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