Ammonia → 6-Methyl-2,4-pyrimidinediamine

A mixture of 50.0 grams (0.348 mole) of 2-amino-4-chloro-6-methylpyrimidine (commercially available) and 100 mL of aqueous 30% ammonia in 400 mL of methanol was placed in a high pressure vessel and heated to 130°-165° C. under a pressure of 140°-250 psig, where it was stirred for 13 hours. After this time, the reaction mixture was allowed to cool to ambient temperature. The reaction vessel was then opened and the reaction mixture was removed. The reaction vessel was washed with 200 mL of methanol, and the wash was combined with the reaction mixture. The combination was concentrated under reduced pressure to a residual solid. The solid was then stirred for 2 hours at ambient temperature with 100 mL of aqueous 30% ammonia. The mixture was cooled to 0° C., and the solid was collected by filtration. The solid was dried, yielding 40.8 grams of 2,4-diamino-6-methylpyrimidine. The NMR spectrum was consistent with the proposed structure.

1. customwas placed in a high pressure vessel
2. temperatureheated to 130°-165° C. under a pressure of 140°-250 psig, where it
3. customthe reaction mixture was removed
4. washThe reaction vessel was washed with 200 mL of methanol
5. concentrationThe combination was concentrated under reduced pressure to a residual solid
6. stirringThe solid was then stirred for 2 hours at ambient temperature with 100 mL of aqueous 30% ammonia
7. temperatureThe mixture was cooled to 0° C.
8. filtrationthe solid was collected by filtration
9. customThe solid was dried

ORDレコード

ord-5b1e6a49a2924e3383b5caea867259df

出典データセット

uspto-grants-1996_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05587379