反応 #565304

ord-f2994ca8f3984b3c9380f9c80433af2f

反応条件

温度
-40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他equipped with a funnel
  2. 2
    その他to flush through the funnel
  3. 3
    その他was then brought up to room temperature
  4. 4
    workup.STIRRINGkept stirring for four hours

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06641833B2uspto-grants-2003_11