Triethylamine → 3-Ethyl 5-methyl 6-(difluoromethyl)-4-(2-methylaziridinyl)-2-(trifluoromethyl)-3,5-pyridinedicarboxylate

A mixture of 2.5 g (0.0059 mol) of product of Example 81, 0.6 g (0.0059 mol) of triethylamine and 0.25 g of 5% Pd/C (50% water coated) in 100 ml of ethanol was hydrogenated (446 kPa) for 18 hours at 50° C. The mixture was then filtered through celite and concentrated in vacuo to remove the ethyl alcohol. The residue was poured into water, and extracted with diethyl ether. The ether extract was washed with water, then dried over MgSO4. The dry ether phase was then concentrated in vacuo to yield 2.00 g of a yellow solid. This solid was then recrystallized in hexane to yield 1.28 g (56%) of product as a tan solid; mp 61° C.

1. customfor 18 hours
2. customat 50° C
3. filtrationThe mixture was then filtered through celite and
4. concentrationconcentrated in vacuo
5. customto remove the ethyl alcohol
6. additionThe residue was poured into water
7. extractionextracted with diethyl ether
8. extractionThe ether extract
9. washwas washed with water
10. dry with materialdried over MgSO4
11. concentrationThe dry ether phase was then concentrated in vacuo

ORD-Eintrag

ord-4ae675b5b4994057b63396abb7bc07d0

Quelldatensatz

uspto-grants-1987_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04698093