Nitrogen → 3-Piperidin-1-yl-pyrrolidin-2-one
反応式
C([O:3][C:4](=O)[CH:5]([N:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)[CH2:6][C:7]#[N:8])C.N#N>CO>[N:9]1([CH:5]2[CH2:6][CH2:7][NH:8][C:4]2=[O:3])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1参加物
4
反応条件
- 温度
- 50 °C
実験手順
Purge a mixture of 3-cyano-2-piperidin-1-yl-propionic acid ethyl ester (2.36 g, 11.2 mmol) and PtO2 hydrate (0.400 g) in methanol (40 mL) with N2 and stir under 50 psi of H2 at 50° C. for 16 hours. Cool the reaction and filter through hyflo. Remove the solvent from the filtrate in vacuo to afford crude product and purify with a 0 to 10% methanol in CH2Cl2 gradient to afford 1.11 g (59%) of the titled product. Rf=0.18 (9/1 CH2Cl2/methanol). ES MS (m/z): 169 (M+).
後処理
- customPurge
- temperatureCool
- customthe reaction
- filtrationfilter through hyflo
- customRemove the solvent from the filtrate in vacuo
- customto afford crude product
- custompurify with a 0 to 10% methanol in CH2Cl2 gradient
出典と根拠
- ORDレコード
- ord-3163660fa874447cb73b2b80c66e26e0
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07994176B2
反応ノート
読み込み中…