Water → 5-(Trifluoromethyl)isoxazol-3-ylamine

In methanol (15 ml) was dissolved 5-trifluoromethyl-3-(2-(methoxycarbonyl)benzoyl)aminoisoxazole (1.57 g, 0.0050 mole) and 90% hydrazine hydrate (0.42 g, 0.0075 mole) was added to the solution. It was allowed to stand to room temperature for 46 hours. Water (30 ml) was added to it and the mixture was stirred at room temperature for 15 minutes. Crystals were filtered off. The filtered off crystals were washed repeatedly with methylene chloride (45 ml) and the filtrate was extracted with these washings. The filtrate was further extracted with methylene chloride (45 ml×2) and the solvent was distilled off from the combined extract at atmospheric pressure by using a distillation apparatus equipped with a fractionating column packed with glass raschig rings (15 mm in diameter, 200 mm in length). The residue was purified by column chromatography on silica gel to give the title compound. Yield: 0.714 g (93.9%).

1. additionwas added to the solution
2. filtrationCrystals were filtered off
3. filtrationThe filtered off crystals
4. washwere washed repeatedly with methylene chloride (45 ml)
5. extractionthe filtrate was extracted with these washings
6. extractionThe filtrate was further extracted with methylene chloride (45 ml×2)
7. distillationthe solvent was distilled off from the
8. extractioncombined extract at atmospheric pressure
9. customequipped with a fractionating column
10. customThe residue was purified by column chromatography on silica gel

ORDレコード

ord-4de688e69c154f18879b96a5075382a7

出典データセット

uspto-grants-1989_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04797492