HRID1091513
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
Isopropenyl [4-(trifluoromethyl)pyridin-2-yl]carbamate (1.2 g, 5.0 mmol) was suspended in CHCl3 (20 mL) and treated with m-CPBA (841 mg, 5.0 mmol). The reaction was stirred at rt overnight. The reaction was quenched with satd. NaHCO3 and extracted with CHCl3. The organic layer was dried (MgSO4) and concentrated. The crude residue was purified over silica using CH2Cl2 as the eluting solvent. An amber oil was collected (620 mg, 47%); 1H-NMR (DMSO-d6) δ 10.2 (s, 1H), 8.56 (d, J=6.9 Hz, 1H), 8.25 (d, J=2.6 Hz, 1H), 7.52 (ddd, dd, J1=6.8 Hz, J2=2.5 Hz, J3=0.6 Hz, 1H), 4.85 (q, J=1.2 Hz, 1H), 4.80 (d, J=1.2 Hz, 1H), 1.94 (d, J=0.4 Hz, 3H).
WORKUP
后处理
- customThe reaction was quenched with satd
- extractionNaHCO3 and extracted with CHCl3
- dry with materialThe organic layer was dried (MgSO4)
- concentrationconcentrated
- customThe crude residue was purified over silica
- customAn amber oil was collected (620 mg, 47%)