HRID1497908
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
To a solution of diethyl 3-hydroxycyclobutane-1,1-dicarboxylate (159) (649 mg, 3 mmol) in DCM (7 mL) was added PCC (1.37 g, 6.3 mmol) and the mixture was stirred for 4 hours at room temperature. The product was filtered through a silica gel plug and the residue was purified using column chromatography with hexanes/ethyl acetate as eluent to yield diethyl 3-oxocyclobutane-1,1-dicarboxylate (160). 1H NMR (400 MHz, CD2Cl2) δ 4.28 (q, J=7.2 Hz, 4H), 3.63 (s, 4H), 1.31 (t, J=7.2 Hz, 6H). MS m/z 215.1 (M+1)+.
WORKUP
后处理
- filtrationThe product was filtered through a silica gel plug
- customthe residue was purified