HRID1685374
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 stirred solution of (S)-3-isopropyl-6-phenyldihydropyrimidine-2,4(1H,3H)-dione from Step B (310 mg, 1.34 mmol) in THF (6 mL) at 0° C. was added NaH (45.0 mg of a 60% dispersion in oil, 1.87 mmol). After 15 min, methyl bromoacetate (0.202 mL, 2.14 mmol) was added and the mixture was stirred at ambient temperature for 16 h. NaOH (4.00 mL of a 1M solution) was added and the mixture was stirred at ambient temperature for 2 h. A 10% citric acid solution (20 mL) was added and the mixture was extracted with CH2Cl2 (3×20 mL). The combined CH2Cl2 extracts were dried over Na2SO4, filtered, and concentrated in vacuo to provide the title compound. MS: m/z=291 (M+1).
WORKUP
后处理
- stirringthe mixture was stirred at ambient temperature for 2 h
- extractionthe mixture was extracted with CH2Cl2 (3×20 mL)
- dry with materialThe combined CH2Cl2 extracts were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo