Reaction #81530

ord-310edeb4ef7b440795de98777deca484

Conditions

Temperature
-10°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Otherin 30 minutes
  2. 2
    TemperatureThe mixture was maintained
  3. 3
    workup.STIRRINGunder stirring at -10° C. for 2 hours and subsequently at 0° C. for 15 hours
  4. 4
    Otherin 30 minutes

Procedure

A solution of 5.74 g isobutylchloroformiate (42 mmol) in 50 ml THF was slowly added drop by drop in 30 minutes to a mixture containing 4.57 g traumatic acid (20 mmol) and 4.26 g triethylamine (42 mmol) in 150 ml anhydrous THF under stirring at -10° C. The mixture was maintained under stirring at -10° C. for 2 hours and subsequently at 0° C. for 15 hours. 3.5 g ethanolamine were slowly added drop by drop in 30 minutes.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05618842uspto-grants-1997_04