Reaction #2027415

Reaction equation

isobutyraldehyde

1,4-dichloro-2,3-butanediol

sulfuric acid

→

2-Isopropyl-4,5-dichloromethyl-1,3-dioxolane

Solvents

EDC

Conditions

Workup

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

Procedure

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