Water → 2-Oxo-4,5,5-trimethyl-3-thiazoline oxime

8.3 g. (0.12 mol) of hydroxylamine hydrochloride were dissolved in 50 ml. of water and treated with 10.1 g. (0.12 mol) of sodium hydrogen carbonate. This solution (pH 6-7) was added with stirring at room temperature to a solution of 14.3 g. (0.1 mol) of 3-methyl-3-thiocyanato-2-butanone in 100 ml. of ethanol. The temperature of the mixture rose rapidly to 37° C. The mixture was then stirred for 1 hour, 120 ml. of the solvent were then distilled off at 50° C. in vacuo. The residue was extracted three times with 100 ml. of ether each time. The organic phase was washed with a small amount of water, dried over sodium sulfate and concentrated until crystallization began. After cooling, the crystal sludge was treated with 10 ml. of hexane. The crystals were filtered off under suction, washed with ether/hexane (2:1) and dried to yield 2-oxo-4,5,5-trimethyl-3-thiazoline-oxime, m.p. 151°-153° C.

1. customrose rapidly to 37° C
2. stirringThe mixture was then stirred for 1 hour
3. distillationof the solvent were then distilled off at 50° C. in vacuo
4. extractionThe residue was extracted three times with 100 ml
5. washThe organic phase was washed with a small amount of water
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated until crystallization
8. temperatureAfter cooling
9. additionthe crystal sludge was treated with 10 ml
10. filtrationThe crystals were filtered off under suction
11. washwashed with ether/hexane (2:1)
12. customdried

ORD record

ord-0ec2f2173ab640f7aa1b1aa7def0c7c3

Source dataset

uspto-grants-1981_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04255436