- Chlorotrimethylsilane (2.7 g, 25mmol) (1) (CAUTION) is added to a solution of lithium bromide (1.74g, 20mmol) in dry acetonitrile (20 ml) (2) with good stirring under a nitrogen atmosphere.
- Cinnamyl alcohol (1.34 g, lOmmol) is then added and the reaction mixture heated under reflux for 12 hours.
- The progress of the reaction is monitored by t.l.c. on silica gel plates with hexane as the eluant.
- On completion of the reaction (12 hours), the reaction mixture is taken up in ether (50 ml), washed successively with water (2 x 25 ml), sodium hydrogen carbonate solution (10%, 50 ml) and finally brine, and dried over anhydrous sodium sulphate.
- Evaporation of the ether affords the pure bromide in 93 per cent yield.
- The product may be recrystallised from ethanol and has m.p. 31-32 °C; CAUTION this compound is lachrymatory.
Notes to keep in mind:
1. Chlorotrimethylsilane is distilled over sodium
hydroxide pellets.
2. Acetonitrile is purified and stored over molecular sieves.
No comments:
Post a Comment
We specialize in producing high value chemicals. Besides our regular products, we strive to develop new products based on customer’s requirements. Our R&D center plays crucial role in handling complex chemistries and developing newer technologies. We respect intellectual property rights and have confidentiality agreement with various multi national companies. We undertake contract manufacturing of fine chemicals and advance intermediates of API’s.