tert-Butyl 4-(cyanomethylidene)piperidine-1-carboxylate → tert-Butyl 4-(cyanomethyl)piperidine-1-carboxylate
反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11](=[CH:14][C:15]#[N:16])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(O)C.[Pd]>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([CH2:14][C:15]#[N:16])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]参加物
4
実験手順
Add 4-cyanomethylenepiperidine-1-carboxylic acid t-butyl ester (5.39 g, 24.25 mmol) in ethanol (160 mL) to a suspension of 5% palladium on charcoal (0.69 g) in ethanol (20 mL) and hydrogenate at room temperature with agitation at 60 psi for 6 hr. Filter the mixture through celite and evaporate the solvent in vacuo to give 4-cyanomethylpiperidine-1-carboxylic acid t-butyl ester as an oil which solidifies on standing to give a solid (5.43 g, 99.8%). MS (m/z): 247 (M+Na).
後処理
- filtrationFilter the mixture through celite
- customevaporate the solvent in vacuo
出典と根拠
- ORDレコード
- ord-2724c4bbb86a488a8ab4f6ca7bf613da
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07910588B2
反応ノート
読み込み中…