Triethylamine → HCID 21568316, compound

Participants

Reaction Steps

To a solution of 1-vinylphosphindoline 1-oxide (6.4g, 36.0 mmol) in carbon tetrachloride (80 ml) was added N-bromosuccinimide (6.8g, 38.6 mmol) and the two phase mixture stirred under reflux whilst being irradiated with a 500 watt mercury lamp. After 15 mins the solution was washed with water, the washings were extracted with chloroform and the combined organic extract was dried and evaporated to give a light yellow oil. A p.m.r. spectrum of this indicated that it was 3-bromo-1-vinylphosphindole 1-oxide. This material was heated under reflux with triethylamine (10 ml) for 5 mins, cooled, and the precipitated hydrobromide filtered off. The benzene filtrate was washed with water, dried and evaporated. Distillation gave an oil (5.8g, b.p. 170°/0.01 min), g.l.c. of which showed it to be about 90% pure.

Provenance & Evidence