HRID2263509

反应详情

EQUATION

反应方程式

HRID 2263509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-(2,3-dichlorophenyl)-1,2,3,6-tetrahydropyridine (0.49 g, 2.15 mmol), platinum oxide (0.11 g) and hydrochloric acid (0.1 ml, conc) in methanol (30 ml) was hydrogenated at 50 psi for 1 h under hydrogen gas. The reaction mixture was filtered through a pad of celite and the filtrate was concentrated and evaporated to dryness. Aqueous sodium carbonate (10%, 50 ml) was added. The aqueous phase was extracted with ethylacetate (3×30 ml) and the combined organic phases was dried (MgSO4), filtered and evaporated to dryness. Yield: 0.17 g. MS m/z (rel. intensity, 70 eV) 230 (M+, 22), 229 (24), 228 (35), 196 (30), 194 (bp).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through a pad of celite
  2. concentrationthe filtrate was concentrated
  3. customevaporated to dryness
  4. additionAqueous sodium carbonate (10%, 50 ml) was added
  5. extractionThe aqueous phase was extracted with ethylacetate (3×30 ml)
  6. dry with materialthe combined organic phases was dried (MgSO4)
  7. filtrationfiltered
  8. customevaporated to dryness