Ethyl alpha-benzylacetoacetate → HCID 136026728, 화합물

HRID 1673577노트

반응식

HRID 1673577 반응식
F[B-](F)(F)F.[C:6](=[NH:11])([O:8][CH2:9][CH3:10])[NH2:7].[CH2:12]([CH:19]([C:25](=O)[CH3:26])[C:20](OCC)=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C[O-].[Na+]>CO>[CH2:12]([C:19]1[C:20](=[O:21])[NH:11][C:6]([O:8][CH2:9][CH3:10])=[N:7][C:25]=1[CH3:26])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 246929Ethyl alpha-benzylacetoacetateHCID 10942334Sodium MethoxideHCID 86622837Ethyl imidocarbamate tetrafluoroborate

생성물 1

HCID 136026728HCID 136026728, 화합물수율 24.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of ethyl imidocarbamate tetrafluoroborate (2.4 g) and ethyl 2-benzyl-3-oxobutanoate (1 g) in methanol (20 mL) was added sodium methoxide (28% methanol solution, 5.25 mL), and the mixture was stirred for 12 hr. The reaction mixture was concentrated, and the residue was dissolved in water. The solution was weakly acidified with acetic acid, extracted with ethyl acetate, washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was crystallized from diisopropyl ether to give the title compound (0.27 g, 24%) as a colorless solid.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in water
  3. extractionextracted with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was crystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-566560f9cf9142f79cc313baa0afc98c
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998968B2

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