4-Chloro-6-hydrazinyl-2-(methylsulfanyl)pyrimidine → 2,6-Bis(methylthio)-6-hydrazinylpyrimidine

温度

20 °C

A mixture of the known compound 6-chloro-4-hydrazinyl-2-methylthiopyrimidine (15 g, 0.079 mole) and 21 g (0.1 mole) of sodium methyl mercaptide in 250 ml of methanol was heated at reflux for about 16 hours, and was then allowed to cool to about 20° C. The solid precipitate was separated by filtration, washed with methanol and water and dried. The filtrate was evaporated to provide a solid residue. This residue was then washed thoroughly with water and combined with the precipitate. The solids were dissolved in 500 ml of acetic acid, and the solution was treated with decolorizing charcoal, and filtered. The filtrate was cooled and treated with ammonium hydroxide until it was slightly basic. The precipitate was collected by filtration, providing 10.5 g (65%) of 2,6-bis(methylthio)-6-hydrazinylpyrimidine, m.p. 120°-125° C.

1. temperaturewas heated
2. temperatureat reflux for about 16 hours
3. customThe solid precipitate was separated by filtration
4. washwashed with methanol and water
5. customdried
6. customThe filtrate was evaporated
7. customto provide a solid residue
8. washThis residue was then washed thoroughly with water
9. dissolutionThe solids were dissolved in 500 ml of acetic acid
10. additionthe solution was treated with decolorizing charcoal
11. filtrationfiltered
12. temperatureThe filtrate was cooled
13. additiontreated with ammonium hydroxide until it
14. filtrationThe precipitate was collected by filtration

ORDレコード

ord-f8f6c6431a4447a690ace35440116344

出典データセット

uspto-grants-1985_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04528288