Pyridine → 2,2-Dibromopropyl carbonochloridate

温度

20 °C

16 ml (0.22 mol) of liquid phosgene are condensed into 33 g (0.15 mol) of 2,2-dibromopropanol in 150 ml of CH2Cl2, at -20° C, and 12 ml (0.15 mol) of pyridine in 15 ml of CH2Cl2 are then added slowly dropwise at -20° C to -5° C and the mixture is stirred for a further 2 hours at 20° C. The solution is washed, at 0° C, with water, 5% strength sulphuric acid and H2O and dried (Na2SO4) and the solvent is stripped off (46.1 g of crude product). Vacuum distillation gives 36.3 g (86%) of 2,2-dibromopropoxycarbonyl chloride as a colorless liquid. Boiling point12 = 81°-86° C.

1. washThe solution is washed, at 0° C, with water, 5% strength sulphuric acid and H2O
2. dry with materialdried (Na2SO4)
3. distillationVacuum distillation

ORDレコード

ord-91608cc15eb1460282ecbe32fca775a7

出典データセット

uspto-grants-1978_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04111933