Benzylamine → Acetoacetobenzylamide

反応式

[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

参加物

実験手順

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%).

後処理

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

出典と根拠

ORDレコード: ord-44680089c2304a02bd1b3d79ce4a32f4
出典データセット: uspto-grants-2016_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09403801B2

反応ノート

読み込み中…

参加物

反応物 2

HCID 7504Benzylamine

HCID 12661Diketene

生成物 1

HCID 70159Acetoacetobenzylamide収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

後処理

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

出典と根拠

ORDレコード: ord-44680089c2304a02bd1b3d79ce4a32f4
出典データセット: uspto-grants-2016_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09403801B2

反応ノート

読み込み中…