반응식
[CH:1]([N:3]1[CH2:7][CH2:6][CH2:5][C:4]1=[O:8])=[CH2:2].[O-]Cl.[Na+].[N:12]1([CH2:18][CH2:19][CH:20]=[N:21][OH:22])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1>C(Cl)(Cl)Cl>[N:12]1([CH2:18][CH2:19][C:20]2[CH2:2][CH:1]([N:3]3[CH2:7][CH2:6][CH2:5][C:4]3=[O:8])[O:22][N:21]=2)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1참가 물질
반응 조건
- 온도
- 0 °C
실험 절차
To a solution of 646 μL (1.5 equivalent) of N-vinyl-pyrrolidin-2-one in 5 mL of chloroform, a biphasic solution of 7.4 mL (3.2 equivalents) of 13% Clorax (NaOCl) and a solution of 629.3 mg (4.03 mmol) of 3-piperidin-1-yl-propionaldehyde oxime compound prepared in Example 2 in 5 mL of chloroform were added slowly over 15 minutes with cooling to 0° C. and stirring vigorously. After reacting at room temperature overnight, the reaction mixture was extracted with chloroform three times, washed with a saturated aqueous solution of sodium carbonate twice following water once, dried over sodium sulfate, filtered and then concentrated under reduced pressure. The concentrate was purified by separation with silica gel column chromatography using chloroform/methanol (30:1) as eluent to obtain 477.4 mg (45% yield) of 1-[3-(2-piperidin-1-yl-ethyl)-4,5-dihydro-isoxazol-5-yl]-pyrrolidin-2-one. Subsequently, 1:1 acid addition salt with oxalic acid was obtained from the diethyl ether solution.
후처리
- extractionthe reaction mixture was extracted with chloroform three times
- washwashed with a saturated aqueous solution of sodium carbonate twice following water once
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe concentrate was purified by separation with silica gel column chromatography
출처 및 근거
- ORD 기록
- ord-c215c43c539b429eb0c01714f31ab002
- 출처 데이터셋
- uspto-grants-2004_07
- 특허 번호
- US06759419B2
연결된 노트
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