Sodium hydride → HCID 14612522, 화합물

HRID 1031580노트

반응식

HRID 1031580 반응식
[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]

참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 178471998HCID 178471998, 화합물

생성물 1

HCID 14612522HCID 14612522, 화합물수율 94.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-890515fef6614f90acff898cb2bbe266
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04954507

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