Phosphorus tribromide → 4-bromomethyl-5-chloro-3-difluoromethyl-1-methyl-1H-pyrazole

温度

-10 °C

A solution of 2.0 g (10.0 mmoles) of (5-chloro-3-difluoromethyl-1-methyl-1H-pyrazol-4-yl)-methanol dissolved in 50 ml of diethyl ether was cooled to −10° C. Thereto was added 1.0 g (3.5 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature overnight to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into ice water, followed by extraction with diethyl ether. The resulting organic layer was washed with an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein, to obtain 2.6 g (yield: 100.0%) of 4-bromomethyl-5-chloro-3-difluoromethyl-1-methyl-1H-pyrazole.

1. customto give rise
2. customto a reaction
3. customAfter the completion of the reaction
4. extractionfollowed by extraction with diethyl ether
5. washThe resulting organic layer was washed with an aqueous sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThe resulting solution was subjected to vacuum distillation
8. customto remove the solvent

ORDレコード

ord-b1a2d528b6d241c1963d344d13d6fea5

出典データセット

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07833939B2