HRID62277

反应详情

EQUATION

反应方程式

HRID 62277 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The (E)-4-chloro-5-methoxy-2-(4-((trifluoromethyl)thio)benzylidene)-2,3-dihydro-1H-inden-1-one 176 (75 mg, 0.195 mmol) was dissolved in methanol 25 ml to which was added Pt/c 40 mg and the reaction stirred under H2 balloon for 6 h. The reaction was filtered through celite bed and washed with excess methanol. The organic layer was concentrated to get the crude, which was purified by flash chromatography using 100-200 mesh silica gel. The final compound 177 was eluted at 20% ethylacetate in hexane as half white coloured solid. 1H NMR (400 MHz, CDCl3) δ ppm 7.69 (d, 1H), 7.58 (d, 2H), 7.29 (d, 2H), 6.98 (d, 1H), 3.99 (s, 3H), 3.38 (dd, 1H), 3.18 (dd, 1H), 2.99 (m, 1H), 2.73 (m, 1H); MS-ES+386.8.

WORKUP

后处理

  1. additionwas added Pt/c 40 mg
  2. filtrationThe reaction was filtered through celite bed
  3. washwashed with excess methanol
  4. concentrationThe organic layer was concentrated
  5. customto get the crude, which
  6. customwas purified by flash chromatography
  7. washThe final compound 177 was eluted at 20% ethylacetate in hexane as half white coloured solid