HRID2416543
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of the Dess-Martin reagent (1.59 g, 3.75 mmol) and 3-[4-(2-pyrimidinyl)phenyl]-2-propyn-1-ol (525 mg, 2.50 mmol, prepared as described in Reference Example 239) in dichloromethane (15 mL) was stirred at room temperature for 30 min. Aqueous 10% Na2S2O3 (25 mL) and aq. sat. NaHCO3 (15 mL) were added, the mixture was stirred for 5 min, the layers were separated, and the aqueous layer was extracted with dichloromethane (10 mL). The combined organic layers were dried (MgSO4) and concentrated to provide 465 mg (89%) of the title compound as a yellow solid. MS 209 (M+H)+.
WORKUP
后处理
- stirringthe mixture was stirred for 5 min
- customthe layers were separated
- extractionthe aqueous layer was extracted with dichloromethane (10 mL)
- dry with materialThe combined organic layers were dried (MgSO4)
- concentrationconcentrated