Hydrochloric Acid → 5,5-Bis(bromomethyl)-1,3-dioxane

Temperature

50 °C

A suspension of 26.2 g of 2,2-bis(bromomethyl)-1,3-propanediol, 50 ml of concentrated hydrochloric acid and 50 ml of 38% formaldehyde was stirred in a 50° C. oil bath overnight, then cooled to room temperature and filtered. The filtrate was extracted with three 100 ml portions of ether. The ether extracts were combined, washed with water, dried and evaporated to an oil. A small amount of solid which formed was removed by filtration and washing with ether. The combined filtrate and wash was evaporated under reduced pressure, giving 26.9 g of 5,5-bis(bromomethyl)-1,3-dioxane as a clear oil.

1. temperaturecooled to room temperature
2. filtrationfiltered
3. extractionThe filtrate was extracted with three 100 ml portions of ether
4. washwashed with water
5. customdried
6. customevaporated to an oil
7. customA small amount of solid which formed
8. customwas removed by filtration
9. washwashing with ether
10. washThe combined filtrate and wash
11. customwas evaporated under reduced pressure

ORD record

ord-82cba01676cb4793ac099a7a4f8db9c3

Source dataset

uspto-grants-1990_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04937358