反应 #1470439

ord-5a0dacec4ac64f00a0b4a398b5bbb49e

反应方程式

O=C1CCC(=O)O1
Succinic anhydride
CC(C)c1cccc(C(C)C)c1O
2,6-diisopropylphenol
CC(C)c1cccc(C(C)C)c1OC(=O)CCC(=O)O
2,6-diisopropylphenyl hydrogen succinate
收率 80.2%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他solvents were removed under vacuum
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in water
  3. 3
    workup.ADDITIONadded to an iced solution of dilute hydrochloric acid
  4. 4
    过滤The precipitated product was filtered
  5. 5
    其他recrystallized from ethanol-water

实验过程

Succinic anhydride (14 g, 140 mmol) and dimethylaminopyridine (0.02 g, 0.16 mmol) were added to a solution of 2,6-diisopropylphenol (20.8 ml, 112 mmol) in triethylamine (50 ml) under nitrogen. After 16 hr at room temperature, solvents were removed under vacuum. The residue was dissolved in water and added to an iced solution of dilute hydrochloric acid. The precipitated product was filtered and recrystallized from ethanol-water to yield 25.0 g (80.2% yield) of 2,6-diisopropylphenyl hydrogen succinate (propofol hemisuccinate), mp 101-102° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06254853B1uspto-grants-2001_07