Phosphorus tribromide → 1-Bromo-4-propylcyclohexane

温度

70 °C

142 g (1.0 mol) of trans-4-propylcyclohexanol was stirred at room temperature and 136 g (0.5 mol) of PBr3 was added drop-wise. The reaction was exothermic and reached about 80° C. The product of the reaction was stirred over a hot water bath at 70° C. for 1 hour, cooled to room temperature, and poured into ice water to decompose the excess PBr3. The oily layer was separated out and the aqueous layer was extracted with chloroform. The oily layers were combined and washed with water. The chloroform was distilled off the washed mixture. The oily residue was distilled in a vacuum (b.p. 97° C./14 mmHg) to yield 180 g (0.88 mol) of 4-propyl-1-bromocyclohexane.

1. customreached about 80° C
2. temperaturecooled to room temperature
3. customThe oily layer was separated out
4. extractionthe aqueous layer was extracted with chloroform
5. washwashed with water
6. distillationThe chloroform was distilled off the washed mixture
7. distillationThe oily residue was distilled in a vacuum (b.p. 97° C./14 mmHg)

ORDレコード

ord-10dd6f7602a84afc91804180a264b591

出典データセット

uspto-grants-1993_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05238599