Benzylamine → Acetoacetobenzylamide

HRID 1477940

반응식

HRID 1477940 반응식
[CH2:1]=[C:2]1[O:5][C:4](=[O:6])[CH2:3]1.[C:7]1([CH2:13][NH2:14])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(Cl)Cl>[CH2:13]([NH:14][C:4](=[O:6])[CH2:3][C:2](=[O:5])[CH3:1])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

4

반응물 2

HCID 7504BenzylamineHCID 12661Diketene

생성물 1

HCID 70159Acetoacetobenzylamide수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-methyleneoxetan-2-one (60.00 g, 713.69 mmol) in DCM (600 mL) was added phenylmethanamine (91.76 g, 856.43 mmol) dropwise at 0° C. After addition, the reaction mixture was stirred at rt overnight and concentrated in vacuo. The residue was beaten with a mixture of PE and EtOAc (10/1 (v/v), 200 mL) for 1 h and filtered. The filter cake was washed with a mixture of PE and EtOAc (10/1 (v/v), 100 mL) to give the title compound as a yellow solid (136.38 g, 100%).

후처리

  1. additionAfter addition
  2. concentrationconcentrated in vacuo
  3. additionThe residue was beaten with a mixture of PE and EtOAc (10/1 (v/v), 200 mL) for 1 h
  4. filtrationfiltered
  5. washThe filter cake was washed with a mixture of PE and EtOAc (10/1 (v/v), 100 mL)

출처 및 근거

ORD 기록
ord-44680089c2304a02bd1b3d79ce4a32f4
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403801B2

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