Chloromethyl Methyl Ether → HCID 18753057, compound

Temperature

0 °C

To a cold (0° C.), stirred mixture of 3.60 g of dihydroxyacetone dimer and 16 mL of diisopropylethylamine in 40 mL of dichloromethane is added 6.1 mL of chloromethyl methyl ether. The mixture is stirred and allowed to warm slowly to room temperature. After 18 h, the clear solution is partitioned between ether and dilute HCl. The aqueous phase is placed in a continuous extractor and extracted overnight with ether. The combined organic phase is then dried (MgSO4) and concentrated under reduced pressure. Kugelrohr distillation of the residue at ˜0.5 mmHg and 150° C. oven temperature affords 2.79 g of 2,4,8,10-tetraoxaundecan-6-one as a pale yellow oil.

1. stirringThe mixture is stirred
2. temperatureto warm slowly to room temperature
3. customthe clear solution is partitioned between ether and dilute HCl
4. extractionextracted overnight with ether
5. dry with materialThe combined organic phase is then dried (MgSO4)
6. concentrationconcentrated under reduced pressure
7. distillationKugelrohr distillation of the residue at ˜0.5 mmHg and 150° C. oven temperature

ORD record

ord-50b423f40e524d27aa76faf1adfa5a8e

Source dataset

uspto-grants-2004_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06673793B2