HCID 21829171, compound → Pyridine, 2,3,5-trichloro-

A solution was prepared by dissolving 2.5 grams of 2,3,5-trichloro-4-hydrazinopyridine in 25 milliliters of tetrahydrofuran. To this mixture was added ~10 milliliters of 5.25 percent sodium hypochlorite. The mixture was stirred at ~30° C. for about one hour. The mixture was diluted with water and extracted with methylene chloride. The extract was washed with water and the methylene chloride removed by evaporation. The residue, a dark brown oil, was recovered in a yield of 2.1 grams. The crude 2,3,5-trichloropyridine product was sublimed at ~1 millimeter of mercury and ~50° C. The purified product was obtained in a yield of 1.52 grams (72 percent of theoretical). The structure was confirmed by N.M.R.

1. customA solution was prepared
2. extractionextracted with methylene chloride
3. washThe extract was washed with water
4. customthe methylene chloride removed by evaporation
5. customThe residue, a dark brown oil, was recovered in a yield of 2.1 grams
6. customwas sublimed at ~1 millimeter of mercury and ~50° C
7. customThe purified product was obtained in a yield of 1.52 grams (72 percent of theoretical)

ORD record

ord-1d2fe549bcee42c18b0ff0dce246ac38

Source dataset

uspto-grants-1978_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04127575