4-Methylmorpholine → 1,4-Cyclohexanedimethanol

HRID 478122

반응식

HRID 478122 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]1

참가 물질

5

반응물 3

HCID 79724-MethylmorpholineHCID 6422909Phosphorodichloridic acid, hexyl esterHCID 178520956HCID 178520956, 화합물

생성물 1

HCID 77351,4-Cyclohexanedimethanol

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

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

  1. customequipped with a funnel
  2. customto flush through the funnel
  3. customwas then brought up to room temperature
  4. 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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