Ammonia → 5-(Chloromethyl)isoxazole-3-carboxamide

Ammonia was passed into a solution of 10 g (55.56 mmol) of 5-chloromethylisoxazole-3-carbonyl chloride in 100 ml of methylene chloride at 10-15° C. for 1 h, and the mixture was then stirred at room temperature for 1 h. After the solution had been cooled to 0° C., the precipitate was filtered off with suction and washed with a little cold methylene chloride, and the residue was extracted by stirring with water twice to remove ammonium salts. Drying under reduced pressure resulted in 6.58 g of pure product as a pale powder (74% of theory).

1. temperatureAfter the solution had been cooled to 0° C.
2. filtrationthe precipitate was filtered off with suction
3. washwashed with a little cold methylene chloride
4. extractionthe residue was extracted
5. stirringby stirring with water twice
6. customto remove ammonium salts
7. customDrying under reduced pressure

ORD 기록

ord-24ed384826b94109bc700eb6b8178389

출처 데이터셋

uspto-grants-2000_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06114358