4-Methylmorpholine → 1,4-Cyclohexanedimethanol
반응식
[C@H:1]1([CH2:9][OH:10])[CH2:6][CH2:5][C@H:4]([CH2:7][OH:8])[CH2:3][CH2:2]1.CN1CCOCC1.P(Cl)(Cl)(=O)OCCCCCC>C(Cl)Cl>[CH2:3]1[CH:4]([CH2:7][OH:8])[CH2:5][CH2:6][CH:1]([CH2:9][OH:10])[CH2:2]1참가 물질
5
반응 조건
- 온도
- -40 °C
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.
후처리
- customequipped with a funnel
- customto flush through the funnel
- customwas then brought up to room temperature
- stirringkept stirring for four hours
출처 및 근거
- ORD 기록
- ord-f2994ca8f3984b3c9380f9c80433af2f
- 출처 데이터셋
- uspto-grants-2003_11
- 특허 번호
- US06641833B2
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