HRID1896002
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
Into a solution of the Compound of Example 39 (300 mg, 0.91 mmol) in anhydrous CH2Cl2 (10 mL) cooled at −78° C. was dropped diethylaminosulfur trifluoride (144 μL, 1.01 mmol). The reaction mixture was kept at the same temperature for 2 h, then warmed up to r.t., quenched with water and extracted with CH2Cl2. The combined organic layers were washed with brine, dried on Na2SO4 and evaporated to dryness in vacuo to afford a residue, which was purified by automated flash liquid chromatography (Horizon™-Biotage) eluting with Petroleum Ether-EtOAc 7:3, affording the title product (140 mg) as an oil.
WORKUP
后处理
- customquenched with water
- extractionextracted with CH2Cl2
- washThe combined organic layers were washed with brine
- customdried on Na2SO4
- customevaporated to dryness in vacuo
- customto afford a residue, which
- customwas purified by automated flash liquid chromatography (Horizon™-Biotage)
- washeluting with Petroleum Ether-EtOAc 7:3