Dimethyl Sulfate → HCID 19858279, compound

Temperature

100 °C

To 2,2-bis(bromomethyl)propane-1,3-diol (100 g) was added potassium bicarbonate (80 g) and dimethyl sulphate (170 g). The mixture was stirred and heated to 100° C. After about 30 minutes at this temperature the reaction became very vigorous (Care!). After a further 2 hours heating and stirring the mixture had become very viscous. The mixture was cooled, made slightly basic by the addition of sodium bicarbonate, and then extracted with chloroform (4×200 cm3). The chloroform extracts were combined and the solvent removed under reduced pressure to give the crude product. Repeated distillation under reduced pressure gave the pure product (25 g) as a colourless liquid (b.p. 65°-70° C. at 0.1 mmHg).

1. temperatureAfter a further 2 hours heating
2. stirringstirring the mixture
3. temperatureThe mixture was cooled
4. extractionextracted with chloroform (4×200 cm3)
5. customthe solvent removed under reduced pressure
6. customto give the crude product
7. distillationdistillation under reduced pressure

ORD record

ord-8dd18062c5e64115acd6283d92d216cb

Source dataset

uspto-grants-1990_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04916214