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Selenium Dioxide → HCID 14010755、化合物

HRID 255673
ノート
印刷プレビュー

反応式

HRID 255673 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24007Selenium DioxideHCID 20183847HCID 20183847、化合物

生成物 1

HCID 14010755HCID 14010755、化合物収率 72%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-015069a57ef44dec9c5f90e1b7788f77
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04698352

反応ノート

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