HRID595738

反应详情

EQUATION

反应方程式

HRID 595738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (E)-ethyl 3-(2,6-dichloropyridin-3-yl)acrylate (500 mg, 2.032 mmol) in Ethanol (15 mL) was added 10% platinum on carbon (96 mg, 0.049 mmol). The flask was alternately evacuated and filled with hydrogen five times. The solution was stirred under 1 ATM (balloon) of hydrogen for 1 h, then filtered through celite, while washing well with MeOH and EtOAc. The filtrate was concentrated in vacuo to provide the title compound which was used without further purification. 1H NMR δ (ppm) (CHCl3-d): 7.62 (1H, d, J=7.92 Hz), 7.24 (1H, d, J=7.8), 4.15 (2H, q, J=7.15 Hz), 3.05 (2H, t, J=7.35 Hz), 2.69 (2H, t, J=7.35 Hz), 1.31˜1.24 (3H, m). MS (M+H)+: 247.

WORKUP

后处理

  1. customThe flask was alternately evacuated
  2. additionfilled with hydrogen five times
  3. filtrationfiltered through celite
  4. washwhile washing well with MeOH and EtOAc
  5. concentrationThe filtrate was concentrated in vacuo