Réaction #2027415

ord-d019aebf564f4f3c958d6ed5753543a0

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreA three-neck 5-mL flask fitted with a thermometer, mechanical stirrer, addition funnel, condenser and positive nitrogen atmosphere
  2. 2
    Autrethe flask was immersed in an ice bath
  3. 3
    Températureto maintain a reaction temperature of 17°-19° C
  4. 4
    Autrewas then continued at ambient temperature
  5. 5
    Autre(20° C.)
  6. 6
    Autrefor five hours

Mode opératoire

A three-neck 5-mL flask fitted with a thermometer, mechanical stirrer, addition funnel, condenser and positive nitrogen atmosphere was charged with EDC (200 mL), isobutyraldehyde (11.3 g, 0.157 mole), and 1,4-dichloro-2,3-butanediol (25.0 g, 0.157 mole). Concentrated sulfuric acid (23.2 g) was added dropwise to the agitated mixture over thirty minutes, during which time a slight exotherm was noticed and the flask was immersed in an ice bath to maintain a reaction temperature of 17°-19° C. Stirring was then continued at ambient temperature (20° C.) for five hours.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05698718uspto-grants-1997_12