HRID1096808
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 2-(2-ethyl-[1,3]dioxolan-2-yl)fluoroacetic acid methyl ester (1.50 g, 7.80 mmol) and hydroxylamine hydrochloride (1.07 g, 15.6 mmol) were dissolved in pyridine (8 mL). MeONa (30% in MeOH, 3.94 mL, 15.6 mmol) was dropped slowly over 15 min. More pyridine (8 mL) was added. The mixture was stirred for 30 min, then filtered. AcOH (1 mL) was added to the filtrate. The mixture was stirred for 5 min, then the solvents were removed under reduced pressure. Purification by FC (MeOH/CH2Cl2 1:10) yielded the title compound (502 mg, 40%).
WORKUP
后处理
- filtrationfiltered
- additionAcOH (1 mL) was added to the filtrate
- stirringThe mixture was stirred for 5 min
- customthe solvents were removed under reduced pressure
- customPurification by FC (MeOH/CH2Cl2 1:10)