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

1. customis 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 is removed
4. washThe reaction vessel is washed with 200 mL of methanol
5. concentrationThe combination is concentrated under reduced pressure to a residual solid
6. stirringThe solid is then stirred for 2 hours at ambient temperature with 100 mL of aqueous 30% ammonia
7. temperatureThe mixture is cooled to 0° C.
8. filtrationthe solid is collected by filtration
9. customThe solid is dried

ORDレコード

ord-ecd66e4b5d5b49df82bcd22f3da55f3b

出典データセット

uspto-grants-1997_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05622954