1,3-Dibromopropane → HCID 67443024, compound

1,3-dibromopropane (287 ml) was heated to 45° C. and pyrrolidine (23.4 ml) added over 4 hours. The mixture was then cooled to room temperature and evaporated to dryness on a is rotary evaporator. To the residual oil was added water (200 ml) and the small organic lower layer separated. The solution was washed with dichloromethane (20 ml). The aqueous layer was basified by the addition of potassium carbonate (42.8 g) and extracted with dichloromethane (2×80 ml). The combined organic extracts were dried over magnesium sulphate and evaporated to dryness on a rotary evaporator. The residue was triturated by the addition of acetone (30 ml) and stirred overnight. The solid was filtered, washed with acetone (30 ml) and dried in a vacuum oven at 40° C.

1. customevaporated to dryness on a is rotary evaporator
2. additionTo the residual oil was added water (200 ml)
3. customthe small organic lower layer separated
4. washThe solution was washed with dichloromethane (20 ml)
5. additionThe aqueous layer was basified by the addition of potassium carbonate (42.8 g)
6. extractionextracted with dichloromethane (2×80 ml)
7. dry with materialThe combined organic extracts were dried over magnesium sulphate
8. customevaporated to dryness on a rotary evaporator
9. customThe residue was triturated by the addition of acetone (30 ml)
10. filtrationThe solid was filtered
11. washwashed with acetone (30 ml)
12. customdried in a vacuum oven at 40° C.

ORD record

ord-5b6cdcbea38149adabdcfea4f95514cd

Source dataset

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08754240B2