4-Methylmorpholine → 1,4-Cyclohexanedimethanol

HRID 478122

反応式

HRID 478122 の反応式
[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

参加物

5

反応物 3

HCID 79724-MethylmorpholineHCID 6422909Phosphorodichloridic acid, hexyl esterHCID 178520956HCID 178520956、化合物

生成物 1

HCID 77351,4-Cyclohexanedimethanol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
-40 °C

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.

後処理

  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

出典と根拠

ORDレコード
ord-f2994ca8f3984b3c9380f9c80433af2f
出典データセット
uspto-grants-2003_11
特許番号
US06641833B2

関連ノート

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