Homoallyl bromide → Bisbutenyl mercury
反応式
[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]参加物
7
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-c734b09e9cf34009a087b33304658c33
- 出典データセット
- uspto-grants-1993_03
- 特許番号
- US05192616
反応ノート
読み込み中…