Homoallyl bromide → Bisbutenyl mercury
반응식
[CH2:1]([Hg:5][CH2:6][CH2:7][CH:8]=[CH2:9])[CH2:2][CH:3]=[CH2:4].C([Mg]Br)CC=C.BrCCC=C.[Mg]>O1CCCC1.O>[CH:1]([Hg:5][CH:6]=[CH:7][CH2:8][CH3:9])=[CH:2][CH2:3][CH3:4]참가 물질
7
실험 절차
Preparation of bis(3-butenyl)mercury: To a solution of 3-butenylmagnesium bromide, prepared from 25 g of 1-bromo-3-butene (187 mmole) and 5 g of magnesium (208 mmole) in 40 mL of tetrahydrofuran, was added dropwise, at 50° C. with stirring, a solution of 25.2 g of mercuric chloride (93 mmole) in tetrahydrofuran. After stirring for 2 hours at 60° C., the reaction mixture was hydrolyzed with water at 0°-5° C. Organic layer was separated from aqueous layer; the product was distilled to give bisbutenyl mercury in 60% yield. The yield of the desired product was confirmed by gas chromatography (GC) and 1H NMR.
후처리
- additionwas added dropwise, at 50° C.
- stirringAfter stirring for 2 hours at 60° C.
- customOrganic layer was separated from aqueous layer
- distillationthe product was distilled
출처 및 근거
- ORD 기록
- ord-fbc0733cf4d7463da771ea1e33495281
- 출처 데이터셋
- uspto-grants-1992_04
- 특허 번호
- US05104952
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