反应 #1509647

ord-878cfb7faf93462c9aeddc0a5c8513d8

反应方程式

CC(CO)(CO)CO
1,1,1-tris(hydroxymethyl)ethane
COC(C)(C)OC
2,2-dimethoxypropane
O=S(=O)(O)O
sulfuric acid
CC1(CO)COC(C)(C)OC1
(1,4,4-trimethyl-3,5-dioxanyl)methane-1-ol
收率 72.0%

溶剂

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他was changed back to a room temperature
  2. 2
    workup.STIRRINGthe mixture was stirred for 2 hours
  3. 3
    workup.DISTILLATIONAfter acetone was distilled off
  4. 4
    其他a fraction obtained at 70° C. under reduced pressure (1.7 mmHg)
  5. 5
    其他was collected

实验过程

In a three-necked flaks, 1,1,1-tris(hydroxymethyl)ethane (200 g) and 2,2-dimethoxypropane (260 g) were suspended in acetone (150 g), one droplet of concentrated sulfuric acid was added thereto at 0° C., and then the mixture was stirred for 2 hours. The temperature was changed back to a room temperature, and the mixture was stirred for 2 hours. After acetone was distilled off, a fraction obtained at 70° C. under reduced pressure (1.7 mmHg) was collected to obtain (1,4,4-trimethyl-3,5-dioxanyl)methane-1-ol (192 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08927195B2uspto-grants-2015_01