Benzyl Alcohol → HCID 67375539, compound

Participants

Reaction Conditions

Reaction Steps

4.95 g of p-toluenesulfonic acid monohydrate was added to 30.0 g of 3,3-dimethoxypropionitrile, 67.63 g of benzyl alcohol and 100 ml of toluene, and the mixture was stirred at 110° C. for 8 hours. The reaction solution was returned to room temperature, and 5.26 g of triethylamine was added. After stirring for 5 minutes, the reaction solution was transferred to a separating funnel and washed with 200 ml of an aqueous 1 mass % potassium carbonate solution once and then with 200 ml of distilled solution three times. Toluene and the unreacted raw materials were removed by distillation under reduced pressure to obtain 60.6 g of 3,3-dibenzyloxypropionitrile. Thereto, 21.36 g of acetyl chloride was added, and the mixture was stirred at 45° C. for 6 hours. The reaction solution was returned to room temperature, and unreacted acetyl chloride was removed by distillation under reduced pressure. The reaction solution was analyzed by 1H-NMR, as a result, the concentration of 3-chloro-3-benzyloxypropionitrile in the reaction solution was 54.2 mass %.

Provenance & Evidence