Sodium Chloride → HCID 53909514, compound

192 g (1.2 mol) of the obtained 3-hydroxypropoxy methylstyrene and 55 ml of dehydrated and purified pyridine were charged into a 300 ml four-necked flask, and 108 g (0.4 mol) of phosphorus tribromide was dropwise added thereto while maintaining the mixture at -10° C. with dry ice ethanol. After completion of the dropwise addition, the mixture was stirred at room temperature for 15 hours. The reaction mixture was poured into 250 ml of an aqueous sodium chloride solution (20 wt %) and extracted with toluene. The organic layer was washed with water and a 8% sodium hydrogencarbonate aqueous solution and dried over magnesium sulfate. Then, toluene was distilled off under reduced pressure. The solution thereby obtained was subjected to vacuum distillation (b.p. 90° to 91° C./54 Pa) in the presence of DPPH to obtain 3-bromopropoxymethylstyrene as the desired product. The yield was 35%. The obtained solution was analyzed by 1H-NMR and IR spectrum.

1. additionwere charged into a 300 ml four-necked flask
2. additionAfter completion of the dropwise addition
3. extractionextracted with toluene
4. washThe organic layer was washed with water
5. dry with materiala 8% sodium hydrogencarbonate aqueous solution and dried over magnesium sulfate
6. distillationThen, toluene was distilled off under reduced pressure
7. customThe solution thereby obtained
8. distillationwas subjected to vacuum distillation (b.p. 90° to 91° C./54 Pa) in the presence of DPPH

ORD record

ord-6297c76dbdad45ebbac3e2d57675a0d5

Source dataset

uspto-grants-1996_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05518627