Hydrochloric Acid → 1-Fluoro-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-pentan-3-one hydrochloride

37.2 g (0.2 mol) of 1-fluoro-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-butan-3-one were dissolved in 200 ml of dimethylsulphoxide, 11.2 g (0.2 mol) of potassium hydroxide, dissolved in 24 ml of water, were added and 28.4 g (0.2 mol) of methyl iodide were added dropwise at 20° C., whilst cooling. The reaction mixture was subsequently stirred at room temperature for 24 hours and poured onto 1,000 ml of water, the mixture was extracted twice with 200 ml of methylene chloride each time, the combined organic phases were washed five times with 100 ml of water each time and dried over sodium sulphate, the solvent was distilled off, the residue was taken up in 100 ml of acetone, the mixture was filtered and the solvent was distilled off from the mother liquor. The residue was taken up in 150 ml of ethyl acetate, and 14.4 g (0.2 mol) of hydrogen chloride were passed in. Thereafter, the mixture was allowed to crystallise out. 33.8 g (72% of theory) of 1-fluoro-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-pentan-3-one hydrochloride of melting point 142° C. were obtained. ##STR62##

1. additionwere added
2. temperaturewhilst cooling
3. extractionthe mixture was extracted twice with 200 ml of methylene chloride each time
4. washthe combined organic phases were washed five times with 100 ml of water each time
5. dry with materialdried over sodium sulphate
6. distillationthe solvent was distilled off
7. filtrationthe mixture was filtered
8. distillationthe solvent was distilled off from the mother liquor
9. customto crystallise out

ORDレコード

ord-6205ab5362be4bfb9d2caf79a0914b04

出典データセット

uspto-grants-1987_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04715887