反应详情

Chloroformic cyanotert. butyl ester is prepared by reacting cyanotert butanol (10 g, 100 mMole) and pyridine (10 g, 125 mmole) in dichloromethane (150 ml) at about -40° C. together with liquid phosgene (-70° C., 40 ml, 600 mMole). The mixture is allowed to warm to room temperature and stirred over night. It is then extracted with ice cold aqueous hydrochloric acid (1N) washed twice with ice water immediately dried by shaking several times with fresh anhydrous sodium sulfate, the aqueous phases and the sodium sulfate are twice reextracted with a small amount of dichloromethane, and the combined organic phases are evaporated under reduced pressure (20° C. bath) to yield the product (17 g, 100% yield).

1. customat about -40° C.
2. extractionIt is then extracted with ice cold aqueous hydrochloric acid (1N)
3. washwashed twice with ice water
4. customimmediately dried
5. stirringby shaking several times with fresh anhydrous sodium sulfate
6. customthe combined organic phases are evaporated under reduced pressure (20° C. bath)