HRID2208653

反应详情

EQUATION

反应方程式

HRID 2208653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 6-methyl-2-oxo-4-propyl-1,2-dihydropyridine-3-carbonitrile (15.0 g, 85.1 mmol) in methanol (600 mL) and concentrated HCl (15 mL) was added Pd(OH)2 (15.0 g). The mixture was stirred for 48 hours under H2 atmosphere. The reaction mixture was filtered and filtrate was concentrated in vacuo. Ethanol was added to the residue, the resulting precipitate was collected and dried to give the titled compound as a white solid (13.0 g, 60% yield). 1H-NMR (400 MHz, CDCl3) δppm; 11.86 (br. s., 1H), 6.00 (s, 1H), 3.78 (q, J=5.5 Hz, 2H), 3.61 (br. s., 2H), 2.46 (m, 2H), 2.17 (s, 3H), 1.50 (sxt, J=7.4 Hz, 2H), 0.91 (t, J=7.4 Hz, 3H).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. concentrationfiltrate was concentrated in vacuo
  3. additionEthanol was added to the residue
  4. customthe resulting precipitate was collected
  5. customdried