4-Methylmorpholine → 1,4-Cyclohexanedimethanol
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
- customequipped with a funnel
- customto flush through the funnel
- customwas then brought up to room temperature
- 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
反応ノート
読み込み中…