Hydrochloric Acid → 3-[1-(2,4-Dimethoxybenzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid
반응식
O[Li].O.C[O:5][C:6](=[O:27])[CH2:7][CH2:8][C:9]1[C:10](=[O:26])[N:11]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][C:17]=2[O:24][CH3:25])[CH2:12][CH2:13][CH:14]=1.Cl>C1COCC1>[CH3:25][O:24][C:17]1[CH:18]=[C:19]([O:22][CH3:23])[CH:20]=[CH:21][C:16]=1[CH2:15][N:11]1[CH2:12][CH2:13][CH:14]=[C:9]([CH2:8][CH2:7][C:6]([OH:27])=[O:5])[C:10]1=[O:26]참가 물질
반응 조건
- 온도
- 0 °C
실험 절차
11 mg of LiOH.H2O solution (0.26 mmol) was added to 0.75 ml of THF solution containing 58 mg of 3-[1-(2,4-dimethoxy benzyl)-2-oxo-1,2,5,6-tetrahydro pyridine-3-yl]-propionic acid methyl ester (d) (0.17 mmol) in a dropwise manner at 0° C. After the reaction mixture was stirred for 2 hrs at 0° C. and for 1 hr at room temperature, 5% HCl was added to the mixture to pH 2. Then the mixture was extracted three times with 10 ml of ethyl acetate, the organic layer was washed with saturated NaCl solution, dried over anhydrous MgSO4, filtered and concentrated in vacuo. The resulting compound was purified with Silica gel column chromatography with methanol/chloroform (1:10) solvent mixture as an eluant to give 44 mg of the title compound (f1) (yield: 80%).
후처리
- extractionThen the mixture was extracted three times with 10 ml of ethyl acetate
- washthe organic layer was washed with saturated NaCl solution
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe resulting compound was purified with Silica gel column chromatography with methanol/chloroform (1:10) solvent mixture as an eluant
출처 및 근거
- ORD 기록
- ord-fcd0c703113844ce9bca477ba2996bd6
- 출처 데이터셋
- uspto-grants-2010_12
- 특허 번호
- US07846963B2
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