Ethyl alpha-benzylacetoacetate → HCID 136026728、化合物

HRID 1673577ノート

反応式

HRID 1673577 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 136026728HCID 136026728、化合物収率 24.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-566560f9cf9142f79cc313baa0afc98c
出典データセット
uspto-grants-2011_08
特許番号
US07998968B2

反応ノート

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