Hydrogen Bromide → 2-(alpha,alpha,beta,beta-Tetrafluorophenethyl)benzyl bromide

A suspension of 3.3 g. (0.0116 mole) of 2-(α,α,β,β-tetrafluorophenethyl)benzyl alcohol in 15 ml. of 48% hydrobromic acid is stirred and heated on the steam bath for 3 hours. The product crystallizes from the cooled mixture and is collected and dissolved in benzene. Evaporation of the washed and dried benzene extract under reduced pressure and sublimation of the residual solid at 60° C. and 0.05 mm. yields white crystals, m.p. 70°-77° C. A sample for analysis from a previous preparation was purified by column chromatography on silica, eluting the product with benzene-carbon tetrachloride (2:1). The fractions that showed one spot of rf 0.85 on a fluorescent silica, thin layer plate developed with benzene were combined and the solvent evaporated under reduced pressure. The residual solid, m.p. 78°-82° C., was sublimed at 60° C. and 0.05 mm. to yield product, m.p. 80.5°-82° C.

1. additionA suspension of 3.3 g
2. temperatureheated on the steam bath for 3 hours
3. customThe product crystallizes from the cooled mixture
4. customis collected
5. dissolutiondissolved in benzene
6. customEvaporation of the
7. washwashed
8. extractiondried benzene extract under reduced pressure and sublimation of the residual solid at 60° C.
9. customyields white crystals, m.p. 70°-77° C
10. customA sample for analysis from a previous preparation
11. customwas purified by column chromatography on silica
12. washeluting the product with benzene-carbon tetrachloride (2:1)
13. customthe solvent evaporated under reduced pressure
14. customwas sublimed at 60° C.
15. customto yield product, m.p. 80.5°-82° C.

ORDレコード

ord-db9af0ac51ac40e98cc8989b0cc0829a

出典データセット

uspto-grants-1978_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04071570