1,3-Dibromopropane → HCID 85713821, compound

The solution of 0.591 ml (0.473 g, 4.00 mmol) of triethylphosphine in 5 ml of acetonitrile was added to the refluxing solution of 4.04 g (20.0 mmol) of 1,3-dibromopropane in 15 ml of acetronitrile over 1 hr. under argon atmosphere. After the addition was completed, the reaction mixture was refluxed for another 6 hrs. After being cooled, acetonitrile was evaporated, 15 ml of ethyl acetate was then introduced into the residue. After being stored in refrigerator for a couple of hours, the highly hygroscopic white solid was collected by filtration. Yield 1.09 g (85%). 1HNMR(DMSOd-6, ppm): 3.64 (t, J=6.7 Hz, 2 H), 2.36-2.17 (m, 8 H) 2.08-2.02 (m, 2 H), 1.13 (d t, J1=18.2 Hz, J2=7.7 Hz, 1 H).

1. additionAfter the addition
2. temperaturethe reaction mixture was refluxed for another 6 hrs
3. temperatureAfter being cooled
4. customacetonitrile was evaporated
5. addition15 ml of ethyl acetate was then introduced into the residue
6. waitAfter being stored in refrigerator for a couple of hours
7. filtrationthe highly hygroscopic white solid was collected by filtration

ORD record

ord-a677c6a958fc42c0b0d0d7b732c36fba

Source dataset

uspto-grants-2001_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06187572B1