HRID52434

反应详情

EQUATION

反应方程式

HRID 52434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of pyridone 5 (5.1 g, 17.89 mmol) in acetic acid (100 ml) was added 10% Pd--C (0.2 g), and the reaction mixture was hydrogenated (55 Psi) at room temperature overnight. The mixture was then filtered through Celite and the filtrate was evaporated. The residue was thoroughly washed with 10% potassium carbonate, water and dried in vacuo to give compound 6 as a white powder (3.3 g, 95% yield) m.p. 124°-126° C. 1H-NMR (DMSO-d6) δ 7.52 (brs, 1H), 4.45 (q, J=7.2 Hz, 2H), 2.40 (s, 3H), 2.07 (s, 3H), 1.42(t, J=7.2 Hz, 3H). Ms(13eV)m/z(%): 195.0(M+, 100), 165.9(40), 148.9(50), 122.9(80), 121.0(100). Anal. Calcd for C10H13NO3 : C, 61.53; H, 6.71; N, 7.18. Found: C, 61.48; H, 6.63; N, 7.09.

WORKUP

后处理

  1. customat room temperature
  2. customovernight
  3. filtrationThe mixture was then filtered through Celite
  4. customthe filtrate was evaporated
  5. washThe residue was thoroughly washed with 10% potassium carbonate, water
  6. customdried in vacuo