Reaction equation
C(OCCOCCl)(=O)C.[CH:10]([O:13][P:14]([O:19]C(C)C)[O:15][CH:16]([CH3:18])[CH3:17])([CH3:12])[CH3:11]>>[PH:14](=[O:19])([O:15][CH:16]([CH3:18])[CH3:17])[O:13][CH:10]([CH3:12])[CH3:11]Participants
Conditions
- Temperature
- 125 °C
Procedure
A 500 mL three-neck flask was charged with the crude chloromethylether 1 (317 g, 2.00 mol). Triisopropylphosphite (494 mL) was added dropwise through an additional funnel while heating in a 125° C. oil bath and stirring vigorously. Collect 2-chloropropane distillate via short-path head in a dry ice cooled receiver, argon blanket, collected 140 g distillate (theoretical 157 g). Phosphite blanched reaction to yellow, continue heating another 2 h at 125° C. oil bath, then arrange for vacuum distillation using a vacuum pump. Distilled a yellow front cut (140 g, head to 135° C., bottom to 190° C.), then changed to clean receiver. Main fraction was collected at head temperature of 178-187° C. (mostly 185-187° C.) with vacuum unknown at bath temperature of 222-228° C. 258 g of the product 2 was given (47% yield from 1,3-dioxolane).
Workup
- distillationCollect 2-chloropropane distillate via short-path head in a dry ice cooled receiver, argon blanket, collected 140 g distillate (theoretical 157 g)
- customreaction to yellow,
- temperaturecontinue heating another 2 h at 125° C. oil bath
- distillationarrange for vacuum distillation
- distillationDistilled a yellow front cut (140 g, head to 135° C., bottom to 190° C.)
- customMain fraction was collected at head temperature of 178-187° C. (mostly 185-187° C.) with vacuum unknown at bath temperature of 222-228° C
Sources & evidence
- ORD record
- ord-a26f559d1f7e48569a465696f70f09e1
- Source dataset
- uspto-grants-2012_01
- Patent number
- US08088754B2
Linked notes
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