반응식
[CH2:1]=[C:2]([CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]([O:5]CC)=[O:4].[OH-].[K+]>CO>[CH2:1]=[C:2]([CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]([OH:5])=[O:4]참가 물질
4
실험 절차
The ethyl α-methylenebenzenepropanoate of Step 8 (4.6 g, 24.3 mmol) was dissolved in methanol (12 mL) and then reacted with 2N potassium hydroxide (24 mL) solution. The mixture was stirred at room temperature for 4 hours and concentrated by evaporation. The residue was diluted with water and washed with ether. The aqueous layer was acidified to pH 2 with 1N HCl, and then extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated to give the title compound as colorless oil (2.8 g, 66% yield). 1H NMR: 300 MHz spectrum consistent with proposed structure.
후처리
- concentrationconcentrated by evaporation
- additionThe residue was diluted with water
- washwashed with ether
- extractionextracted with ethyl acetate
- dry with materialThe extracts were dried (MgSO4)
- customevaporated
출처 및 근거
- ORD 기록
- ord-7003251b1fd440dababdec12f1aa32e2
- 출처 데이터셋
- uspto-grants-1995_05
- 특허 번호
- US05416119
연결된 노트
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