HRID1092224
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of (R)-2-[4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-6-methyl-5-nitropyrimidin-2-ylamino]-2-(4-fluorophenyl)ethanol (Method 1, 1.0 g, 2.4 mmol) and zinc dust (0.79 g, 12.0 mmol) in the mixture of MeOH:THF (1:1, 70 ml) was slowly added saturated NH4Cl solution (10 ml). After 3 hours, the reaction was treated with saturated aqueous NH4OAc solution (40 ml), and the resulting mixture was stirred for 30 minutes. The reaction was then filtered through a plug of celite with EtOAc (100 ml). The resulting aqueous layer was extracted with EtOAc (2×100 ml), dried, filtered, and concentrated to give (0.8 g, 90%). MS: Calcd.: 383; Found: [M+H]+ 384.
WORKUP
后处理
- filtrationThe reaction was then filtered through a plug of celite with EtOAc (100 ml)
- extractionThe resulting aqueous layer was extracted with EtOAc (2×100 ml)
- customdried
- filtrationfiltered
- concentrationconcentrated
- customto give (0.8 g, 90%)