Piperonyl Bromide- Piperonyl alcohol (101.44g, 0.067 mol) was added portionwise to HBr (49% aq. 100 mL), and the resultant suspension was
allaowed to stand at room temp for 2h. DCM (1L) was then added, and the organic layer seperated. The aq layer was extracted with DCM (3x 800mL), and
the combined organic extract was washed with water (2x500mL) and saturated aq NaHCO3 (3x500mL), dried and concentrated to yield the crude bromide
(123.63g, ca. 85%), which was sued without further purification. An analytical sample was prepared by recrystallisation from light petroleum,
mp 46-48°C (lit. mp 48°C) [NMR]. |