Ethanethiol → Ethiozin

온도

10 °C

A mixture of 230 g (1 mole of 93% active ingredient) of 4-amino-6-t-butyl-3-methylthio-1,2,4-triazin-5-one and 310 g (5 moles) of ethyl mercaptan and 0.5 g of crushed solid KOH was stirred and refluxed onto a 10° C. condenser. The vapors which pass through the condenser (methyl and ethyl mercaptans) were collected in a dry ice or caustic trap. The reaction was continued until thin layer chromatography indicated that the starting material was gone (usually 2-8 hours). The unreacted ethyl mercaptan was then distilled off while ~600 ml of warm (40° C.) water was added at such a rate that the water addition was complete when ~2/3 of the mercaptan had distilled. Distillation was continued until ~100 ml of water distilled at 100° C. The solution was then allowed to cool with rapid stirring. The product crystallized at 60°14 70° C. and at 20° C. was filtered and washed with water, then dried. The final product, 4-amino-6-t-butyl-3-ethylthio-1,2,4-triazin-5-one, was obtained in nearly quantitative yield and contained less than 1% of the starting 3-methylthio compound.

1. customwere collected in a dry ice or caustic trap
2. customusually 2-8 hours
3. distillationThe unreacted ethyl mercaptan was then distilled off while ~600 ml
4. temperatureof warm (40° C.) water
5. additionwas added at such a rate
6. additionthat the water addition
7. distillationhad distilled
8. distillationDistillation
9. distillationdistilled at 100° C
10. temperatureto cool with rapid stirring
11. customThe product crystallized at 60°14 70° C. and at 20° C.
12. filtrationwas filtered
13. washwashed with water
14. customdried

ORD 기록

ord-e6a8f2d259404a228e5ce2b6f2e911d7

출처 데이터셋

uspto-grants-1988_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04783531