反応式
[N+:1]([CH2:3][C:4]([O:6]C)=O)#[C-:2].[NH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1>>[N+:1]([CH2:3][C:4]([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1)=[O:6])#[C-:2]参加物
3
実験手順
Prepared in accordance with Method B with methyl isocyanoacetate (2.46 g, 24.63 mmol) and piperidine (3.22 mL, 37.85 mmol). The reaction mixture was stirred 1 h at RT and then concentrated. The residue was dissolved in dichloromethane (50 mL) and the organic layer was washed with 10% aqueous citric acid (2×25 mL), dried over MgSO4, filtered and evaporated. 2-Isocyano-1-(piperidin-1-yl)ethanone SLA 07116B was obtained as an orange solid (3.13 g, 83% yield).
後処理
- concentrationconcentrated
- dissolutionThe residue was dissolved in dichloromethane (50 mL)
- washthe organic layer was washed with 10% aqueous citric acid (2×25 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-76bf02fcc46c4062b17d23e373a5af76
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08431599B2
関連ノート
読み込み中…