反应详情

Methyl 4-{5-[4-({(4S,5R)-5-[3,5-bis(trifluoromethyl)phenyl]-4-methyl-2-oxo-1,3-oxazolidin-3-yl}methyl)-2-(morpholin-4-yl)pyrimidin-5-yl]-6-methoxypyridin-3-yl}-3,5-dimethylbenzoate (EXAMPLE 34 Step A, 0.051 g, 0.067 mmol) was dissolved in ethanol (0.45 mL). Added hydrazine (0.063 mL, 2.014 mmol) and stirred at 85° C. in a screw cap vial (pressure relief type) under a nitrogen blanket. Once complete, the solvent was removed by rotary evaporation and the crude isolate was partitioned between ethyl acetate and water. Washed the organic twice more with water, then once with brine, dried over sodium sulfate, filtered and evaporated to give an off-white foam as the product. The compound was used without further purification. 1H NMR (CDCl3, 500 MHz): δ 8.16 (s, 1H), 8.00 (d, 1H), 7.88 (s, 1H), 7.73 (s, 2H), 7.49 (s, 2H), 7.35 (s, 1H), 7.26 (d+s, 1H+CHCl3), 5.66 (d, 1H), 4.71 (d, 1H), 4.33 (m, 1H), 4.10 (m, 1H), 4.00 (s, 3H), 3.85 (m, 4H), 3.80 (m, 4H), 2.15 (s, 3H), 2.13 (s, 3H), 1.60 (br, 2H), 0.72 (d, 3H).

1. customcap vial (pressure relief type) under a nitrogen blanket
2. customOnce complete, the solvent was removed by rotary evaporation
3. customthe crude isolate
4. customwas partitioned between ethyl acetate and water
5. washWashed the organic twice more with water
6. dry with materialonce with brine, dried over sodium sulfate
7. filtrationfiltered
8. customevaporated
9. customto give an off-white foam as the product
10. customThe compound was used without further purification