Pentachloropyridine → 2,3,5,6-Tetrachloropyridine

12.76 g (0.05 mol) of pentachloropyridine is dissolved, by heating at 90° C., in 80 ml of dimethylmethanephosphonate. After the addition of 4.1 g (0.063 gram atom) of zinc dust, there is added dropwise to the clear solution in the course of 20 minutes, with vigorous stirring, a solution of 4.26 g (0.08 mol) of ammonium chloride in 15 ml of water. After the addition of the ammonium chloride solution has been completed, stirring is continued for 40 minutes. The reaction mixture obtained is then filtered hot, and the filter residue is washed with 10 ml of dimethylmethanephosphonate. The filtrate is poured into 500 ml of ice water; there is then added 12.5 ml of concentrated hydrochloric acid and the mixture is stirred for 2 hours. The 2,3,5,6-tetrachloropyridine, which has precipitated in the form of white crystals, is subsequently washed with 150 ml of water and dried. In this manner is obtained 10.0 g (90.8% of theory) of 2,3,5,6 -tetrachloropyridine having a melting point of 89° to 90° C. According to gas-chromatographical analysis, the product contains 97.0% of 2,3,5,6-tetrachloropyridine, 0.5% of 2,3,5-trichloropyridine, 0.6% of 2,3,6-trichloropyridine and 1.6% of pentachloropyridine.

1. additionis added dropwise to the clear solution in the course of 20 minutes, with vigorous stirring
2. customThe reaction mixture obtained
3. filtrationis then filtered hot
4. washthe filter residue is washed with 10 ml of dimethylmethanephosphonate
5. additionThe filtrate is poured into 500 ml of ice water
6. additionthere is then added 12.5 ml of concentrated hydrochloric acid
7. stirringthe mixture is stirred for 2 hours
8. customThe 2,3,5,6-tetrachloropyridine, which has precipitated in the form of white crystals
9. washis subsequently washed with 150 ml of water
10. customdried

ORD 기록

ord-c9814b95be1b4f6e90daaf0dbd769fc7

출처 데이터셋

uspto-grants-1981_03

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04259495