反応 #50094

反応方程式

α-allyl-α-isopropyl-3,4-dimethoxy- benzyl cyanide

azobisisobutyronitrile

hydrogen bromide

potassium carbonate

hydrogen bromide

→

crude product

収率 94.0%

5-Bromo-2-(3,4-dimethoxyphenyl)-2- isopropyl valeronitrile

収率 94.0%

溶媒

cyclohexane

n-hexane

反応条件

後処理

1. 1
   洗浄The separated cyclohexane solution of the product was washed with water until neutral pH
2. 2
   その他After drying
3. 3
   その他evaporating the solvent under diminished pressure

実験手順

To a solution of 50 g of α-allyl-α-isopropyl-3,4-dimethoxy- benzyl cyanide and 2 g of azobisisobutyronitrile in 400 ml of cyclohexane (or n-hexane) gaseous hydrogen bromide was introduced for 70 minutes, when, according to GLC, the reaction mixture did not contain the starting allyl derivative. During the introduction of the hydrogen bromide, the reaction temperature raised to 40° C. The reaction mixture was neutralized with 200 ml of 30% solution of potassium carbonate. The separated cyclohexane solution of the product was washed with water until neutral pH. After drying and evaporating the solvent under diminished pressure, the crude product (61.7 g, 94%) was obtained, which could be used without purification in further reaction step.

出典