反応 #517642

反応方程式

methallyl bromide

methallylbromide

trifluoropyruvic acid ethyl ester

ammonium chloride

ethyl acetate

→

2-hydroxy-4-methylene-2-trifluoromethyl-valeric acid ethyl ester

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   温度at boiling heat over two hours
2. 2
   workup.WAITboiled for another hour
3. 3
   温度while being cooled with ice
4. 4
   洗浄the separated ethyl acetate phase is washed with saturated ammonium chloride solution and three times with water
5. 5
   乾燥The solvent is dried (Na2SO4)
6. 6
   濃縮concentrated by evaporation
7. 7
   workup.DISTILLATIONthe residue is distilled in a vacuum

実験手順

1.3 g of anhydrous zinc chloride and 13.2 g of granular manganese are heated to boiling in 100 ml of tetrahydrofuran and boiled with 0.2 ml of methallyl bromide for 30 minutes. Then, the solution of 25 g of methallylbromide and 17 g of trifluoropyruvic acid ethyl ester in 80 ml of tetrahydrofuran is added in drops at boiling heat over two hours and boiled for another hour. Then, it is added to saturated ammonium chloride solution and 300 ml of ethyl acetate while being cooled with ice, stirred for 30 minutes at 0° C., and the separated ethyl acetate phase is washed with saturated ammonium chloride solution and three times with water. The solvent is dried (Na2SO4) and concentrated by evaporation, and the residue is distilled in a vacuum. 17.6 g of 2-hydroxy-4-methylene-2-trifluoromethyl-valeric acid ethyl ester, boiling point 48° C., 1 hPa, is obtained.

出典