反应详情

温度

80 °C

Ethyl 4-((R)-(2,4-difluorophenyl)(4-hydroxy-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxamido)methyl)phenyl(methyl)phosphinate, 20-f, (400 mg, 0.78 mmol) was dissolved in 5 ml of dioxane and treated with 0.5 ml of 5N NaOH. The mixture was heated at 80° C. for one hour. The mixture was then concentrated under vacuum and the residue was diluted with water and washed with ethyl acetate. The aqueous layer was acidified with AcOH and evaporated to dryness. The residue was used for prep-HPLC to afford the product, 20-1, (100 mg, 26%). 1H NMR (300 MHz, CD3OD): δ 8.67 (s, 1H), 8.58 (s, 1H), 7.92 (s, 1H), 7.81 (m, 2H), 7.48 (m, 3H), 7.04 (m, 2H), 6.66 (s, 1H), 6.60 (s, 1H), 1.66 (d, 3H). (M−H)−=484.0.

1. concentrationThe mixture was then concentrated under vacuum
2. additionthe residue was diluted with water
3. washwashed with ethyl acetate
4. customevaporated to dryness
5. customto afford the product, 20-1, (100 mg, 26%)