Chloroacetonitrile → 2-(4-oxopiperidin-1-yl)acetonitrile
반응식
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]1참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-d96a4e9b8c024403a4170b9d176b4a83
- 출처 데이터셋
- uspto-grants-2003_02
- 특허 번호
- US06518265B1
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