HRID1099311

反应详情

EQUATION

反应方程式

HRID 1099311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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, 1 H), 8.56 (d, J=6.9 Hz, 1 H), 8.25 (d, J=2.6 Hz, 1 H), 7.52 (ddd, dd, J1=6.8 Hz, J2=2.5 Hz, J3=0.6 Hz, 1 H), 4.85 (q, J=1.2 Hz, 1 H), 4.80 (d, J=1.2 Hz, 1 H), 1.94 (d, J=0.4 Hz, 3 H).

WORKUP

后处理

  1. customThe reaction was quenched with satd
  2. extractionNaHCO3 and extracted with CHCl3
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated
  5. customThe crude residue was purified over silica
  6. customAn amber oil was collected (620 mg, 47%)