反应详情

To a solution of 2679 g of 6-hydroxy-5-(2-propenyl)-hexanenitrile in 25 l of methylene chloride is added 2681 ml of triethylamine. The mixture is cooled to -10° in an ice salt bath and a solution of 2103 g of methanesulfonyl chloride in 2 l of methylene chloride is added dropwise over 3 h keeping the temperature at -5°. After addition is complete, the mixture is stirred for 3 h in an ice salt bath and then overnight at 10°. The mixture is washed with water, saturated sodium bicarbonate solution, water and then brine, dried over sodium sulfate, evaporated to dryness, and dried at 45°/3 mm Hg (=4.00 mbar) to yield 6-methylsulfonyloxy-5-(2-propenyl)-hexanenitrile.

1. temperatureThe mixture is cooled to -10° in an ice salt bath
2. customat -5°
3. additionAfter addition
4. customovernight
5. customat 10°
6. washThe mixture is washed with water, saturated sodium bicarbonate solution, water
7. dry with materialbrine, dried over sodium sulfate
8. customevaporated to dryness
9. customdried at 45°/3 mm Hg (=4.00 mbar)