Sodium hydride → HCID 14612522、化合物

HRID 1031580ノート

反応式

HRID 1031580 の反応式
[H-].[Na+].[CH2:3]([O:5][C:6](=[O:25])[C:7](=[CH:19][NH:20][C:21]([CH3:24])([CH3:23])[CH3:22])[C:8]([C:10]1[CH:15]=[C:14]([F:16])[C:13]([F:17])=[CH:12][C:11]=1F)=[O:9])[CH3:4]>O1CCOCC1>[CH2:3]([O:5][C:6]([C:7]1[C:8](=[O:9])[C:10]2[C:11](=[CH:12][C:13]([F:17])=[C:14]([F:16])[CH:15]=2)[N:20]([C:21]([CH3:24])([CH3:23])[CH3:22])[CH:19]=1)=[O:25])[CH3:4]

参加物

4

反応物 2

HCID 24758Sodium hydrideHCID 178471998HCID 178471998、化合物

生成物 1

HCID 14612522HCID 14612522、化合物収率 94.6%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

There was added 1.1 g (27 mmoles) of 60% sodium hydride portionwise, at a temperature between 18° C. to 22° C., to a suspension of 7.22 g (21.9 mmoles) of 3-(2,4,5-trifluorophenyl)-3-oxo-2-(((1,1-dimethylethyl)amino)methylene)propanoic acid ethyl ester in 73 mL of anhydrous dioxane. An exothermic reaction occured. After stirring at room temperature during 1 hour, the resulting mixture was evaporated to dryness, and taken up with CH2Cl2 (150 mL) and H2O (200 mL). After decantation the organic layer was dried over MgSO4. Evaporation of dichloromethane gave 6.41 g of an amorphous solid which was washed twice with water to yield 6.08 g of titled compound.

後処理

  1. customAn exothermic reaction
  2. customthe resulting mixture was evaporated to dryness
  3. dry with materialAfter decantation the organic layer was dried over MgSO4
  4. customEvaporation of dichloromethane

出典と根拠

ORDレコード
ord-890515fef6614f90acff898cb2bbe266
出典データセット
uspto-grants-1990_09
特許番号
US04954507

反応ノート

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