Water → 2,3,5,6-Tetrachloropyridine

温度

160 °C

A suspension of 8.22 g (0.075 mol) of tetramethylammonium chloride in 90 ml of dimethylmethanephosphonate is heated for 1 hour at 160° C. It is then cooled to 90° C., and 12.57 g (0.05 mol) of pentachloropyridine and 3 ml of water are added. There is subsequently added portionwise, in the course of 30 minutes, 4.1 g (0.063 gram atom) of zinc dust. After completion of the addition of the zinc dust, the mixture is firstly stirred for 20 minutes and then filtered. The filtrate is poured into a solution of 12.5 ml of concentrated hydrochloric acid in 500 ml of water, and stirring is maintained for 2 hours. After filtration, the filter residue is washed with water and dried to yield 9.1 g (83.9% of theory) of crude 2,3,5,6-tetrachloropyridine which has a melting point of 88° to 89° C. and which contains, according to gas-chromatographical analysis, 91.25% of 2,3,5,6-tetrachloropyridine, 2.66% of 2,3,5-trichloropyridine, 2.59% of 2,3,6-trichloropyridine and 0.5% of pentachloropyridine.

1. temperatureIt is then cooled to 90° C.
2. filtrationfiltered
3. additionThe filtrate is poured into a solution of 12.5 ml of concentrated hydrochloric acid in 500 ml of water
4. stirringstirring
5. temperatureis maintained for 2 hours
6. filtrationAfter filtration
7. washthe filter residue is washed with water
8. customdried

ORDレコード

ord-25af9fc5e190478a97c47d3fec99070d

出典データセット

uspto-grants-1981_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04259495