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

Temperatur

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-Eintrag

ord-0772aa493a1a4cfca08b3322a4c0a576

Quelldatensatz

uspto-grants-1991_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04996337