Sodium ethoxide → HCID 86660090, 화합물

HRID 1843063노트

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HRID 1843063 반응식
[F:1][C:2]([F:10])([C:6]([F:9])([F:8])[F:7])[C:3](=[NH:5])[NH2:4].C(O[CH:14]=[C:15]([C:21](=O)[CH:22]([F:24])[F:23])[C:16]([O:18][CH2:19][CH3:20])=[O:17])C.CC[O-].[Na+]>C(O)C>[F:23][CH:22]([F:24])[C:21]1[C:15]([C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:14][N:4]=[C:3]([C:2]([F:10])([F:1])[C:6]([F:9])([F:8])[F:7])[N:5]=1

참가 물질

5

반응물 3

HCID 2723922Sodium ethoxideHCID 3681554PentafluoropropylamidineHCID 53395411Butanoic acid, 2-(ethoxymethylene)-4,4-difluoro-3-oxo-, ethyl ester

생성물 1

HCID 86660090HCID 86660090, 화합물수율 40%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1.62 g (10 mmol) of 2,2,3,3,3-pentafluoropropanimidamide and 2.22 g (10 mmol) of ethyl 2-(ethoxymethylene)-4,4-difluoro-3-oxobutanoate (for preparation see WO 2005/123690) in 10 ml of ethanol is stirred under reflux for 4 days after adding 0.68 g (10 mmol) of sodium ethylate. Concentration by evaporation in vacuo is then carried out and the residue is taken up in 10 ml of water and extracted twice with 10 ml of ethyl acetate. The organic phases are washed successively with 5 ml of water and 5 ml of saturated sodium chloride solution, dried over sodium sulphate, filtered and concentrated by evaporation in vacuo. Chromatographic purification with a mixture of cyclohexane and ethyl acetate gives 1.26 g of ethyl 4-(difluoromethyl)-2-(pentafluoroethyl)pyrimidine-5-carboxylate (40%) as a white solid.

후처리

  1. temperatureunder reflux for 4 days
  2. concentrationConcentration
  3. customby evaporation in vacuo
  4. extractionextracted twice with 10 ml of ethyl acetate
  5. washThe organic phases are washed successively with 5 ml of water and 5 ml of saturated sodium chloride solution
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated by evaporation in vacuo
  9. customChromatographic purification
  10. additionwith a mixture of cyclohexane and ethyl acetate

출처 및 근거

ORD 기록
ord-e8e5cbbb0aaf4b7ea5b3d1bd852cf67d
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946234B2

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