Reaction #1509647

ord-878cfb7faf93462c9aeddc0a5c8513d8

Solvents

Conditions

Temperature
0°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Otherwas 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
    Othera fraction obtained at 70° C. under reduced pressure (1.7 mmHg)
  5. 5
    Otherwas collected

Procedure

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).

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08927195B2uspto-grants-2015_01