반응 #565304
ord-f2994ca8f3984b3c9380f9c80433af2f
반응 조건
온도
-40°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타equipped with a funnel
- 2기타to flush through the funnel
- 3기타was then brought up to room temperature
- 4workup.STIRRINGkept stirring for four hours
실험 절차
Under an argon stream, 10 g of trans-1,4-cyclohexane dimethanol (CHDM), 15.25 mL (14.03 g) of N-methyl morpholine (NMM), and 50 mL of methylene chloride were transferred into a 250 mL flash equipped with a funnel. The solution in the flask was cooled down to −40° C. with stirring. A solution of 15.19 g of hexyl phosphoro-dichloridate (HOP) in 20 mL of methylene chloride was added through the funnel, and an additional 10 mL of methylene chloride was used to flush through the funnel. The mixture was then brought up to room temperature gradually and kept stirring for four hours.