2-Chlorobenzylamine → HCID 43445075、化合物
反応式
[N:1](=[C:3]([C:9]([CH3:11])=O)[C:4]([O:6][CH2:7][CH3:8])=[O:5])O.[Cl:12][C:13]1[CH:20]=[CH:19][CH:18]=[CH:17][C:14]=1[CH2:15][NH2:16]>C(#N)C>[CH2:7]([O:6][C:4]([C:3]1[N:1]=[C:15]([C:14]2[CH:17]=[CH:18][CH:19]=[CH:20][C:13]=2[Cl:12])[NH:16][C:9]=1[CH3:11])=[O:5])[CH3:8]参加物
4
実験手順
To a solution of 8.5 g of ethyl 2-oximinoacetoacetate in acetonitrile (100 ml) was added 7.5 ml of 2-chlorobenzylamine. The reaction mixture was then refluxed for 4 hours under argon atmosphere. After such time the reaction mixture was then concentrated in vacuo and the residue was triturated with warm ethylacetate for 10 minutes. After allowing to cool down to room temperature the solid was filtered and dried in vacuo to yield 11.3 g of a white powder, MS (ISP) 265.1 (M+H)+.
後処理
- temperatureThe reaction mixture was then refluxed for 4 hours under argon atmosphere
- concentrationAfter such time the reaction mixture was then concentrated in vacuo
- customthe residue was triturated with warm ethylacetate for 10 minutes
- filtrationwas filtered
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-7460c7adaf9049078e767f6f702d0fa5
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07294644B2
反応ノート
読み込み中…