반응식
[O:1]=[C:2]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[C:4](=[O:11])[N:3]1[CH2:12][CH:13]([C:19]1([CH3:24])OCC[O:20]1)[C:14]([O:16][CH2:17][CH3:18])=[O:15].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(C)=O.O>[O:1]=[C:2]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[C:4](=[O:11])[N:3]1[CH2:12][CH:13]([C:19](=[O:20])[CH3:24])[C:14]([O:16][CH2:17][CH3:18])=[O:15]참가 물질
반응물 2
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 80 °C
실험 절차
Ethyl 3-(1,3-dioxo-1,3,4,5,6,7-hexahydro-isoindol-2-yl)-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (866 mg, 2.57 mmol) was dissolved in a a solvent mixture of acetone/water (v/v=5/1), and a catalytic amount of p-toluenesulfonic acid monohydrate (190 mg, 0.76 mmol) was then added to the obtained solution. The resulting mixture was then refluxed at 80° C. for 4 days. After the reaction was completed, the reaction mixture where white solid were formed was washed with water. Acetone was removed by a vacuum evaporation, and the residue was extracted with dichloromethane. The combined organic layer was dried with anhydrous sulfate and then distilled under a reduced pressure in order to remove dichloromethane. The desired product was obtained (421 mg, 56%) by performing column chromatography (eluent: n-hexane/ethyl acetate=3/1). Rf=0.54 (eluent: n-hexane/ethyl acetate=1/1)
후처리
- customthe reaction mixture where white solid were formed
- washwas washed with water
- customAcetone was removed by a vacuum evaporation
- extractionthe residue was extracted with dichloromethane
- dry with materialThe combined organic layer was dried with anhydrous sulfate
- distillationdistilled under a reduced pressure in order
- customto remove dichloromethane
출처 및 근거
- ORD 기록
- ord-d7980a10b9df46969fa9c65469c6ee48
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07094908B2
연결된 노트
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