Chloroacetonitrile → 2-(4-oxopiperidin-1-yl)acetonitrile
反応式
O.Cl.[NH:3]1[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.Cl[CH2:11][C:12]#[N:13].C(N(C(C)C)CC)(C)C>O1CCCC1>[O:9]=[C:6]1[CH2:7][CH2:8][N:3]([CH2:11][C:12]#[N:13])[CH2:4][CH2:5]1参加物
5
実験手順
A suspension of 25.0 g of 4-piperidinone monohydrochloride monohydrate, 11.5 ml of chloroacetonitrile and 57.0 ml of diisopropylethylamine in 250 ml of tetrahydrofuran was refluxed for 10 hours. After the reaction, an insoluble matter was filtered off. The filtrate was added with saturated aqueous sodium hydrogencarbonate solution and extracted with a mixture of ethyl acetate and methanol (10:1). The extract was dried, and the solvent was evaporated to give brown crystals. The crystals were washed with a mixture of ethyl acetate and n-heptane to give 15.7 g of pale brown crystals.
後処理
- temperaturewas refluxed for 10 hours
- customAfter the reaction
- filtrationan insoluble matter was filtered off
- additionThe filtrate was added with saturated aqueous sodium hydrogencarbonate solution
- extractionextracted with a mixture of ethyl acetate and methanol (10:1)
- customThe extract was dried
- customthe solvent was evaporated
- customto give brown crystals
- washThe crystals were washed with a mixture of ethyl acetate and n-heptane
出典と根拠
- ORDレコード
- ord-d96a4e9b8c024403a4170b9d176b4a83
- 出典データセット
- uspto-grants-2003_02
- 特許番号
- US06518265B1
反応ノート
読み込み中…