HRID915904
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 solution of 1-(3-methoxy4-pyridin-2-ylphenyl)-2-nitroethanol (290 mg, 1.06 mmol) in anhydrous dichloromethane (5 mL) was treated with triethylamine (0.24 mL, 1.69 mmol), followed by methanesulfonyl chloride (0.10 mL, 1.27 mmol), 1 hr later, the mixture was partitioned between sat. NaHCO3 (10 mL) and dichloromethane (20 mL). The phases were separated and the aqueous layer was extracted with dichloromethane (3×10 mL). The combined organic layers were dried (MgSO4), filtered and concentrated to afford a yellow solid.
WORKUP
后处理
- customthe mixture was partitioned between sat. NaHCO3 (10 mL) and dichloromethane (20 mL)
- customThe phases were separated
- extractionthe aqueous layer was extracted with dichloromethane (3×10 mL)
- dry with materialThe combined organic layers were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customto afford a yellow solid