HRID991493

反应详情

EQUATION

反应方程式

HRID 991493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7-bromo-2-trifluoroacetyl-1,2,3,4-tetrahydoisoquinoline (G. E. Stokker, Tetrahedron Letters 1996, 37, 5453) (43.4g, 0.14 mol), potassium carbonate (104.3g, 0.75 mol), methanol (1 L) and water (150ml) was heated at reflux for 1 h, then cooled and evaporated in vacuo. Residue was partitioned between water (1 L) and dichloromethane (4×200 ml). Combined extracts were dried (Na2SO4) and evaporated in vacuo to give an oil which was dissolved in hexane. The mixture was filtered and the filtrate evaporated in vacuo to give the title compound as an oil (17.7 g, 60%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 1 h
  3. temperaturecooled
  4. customevaporated in vacuo
  5. customResidue was partitioned between water (1 L) and dichloromethane (4×200 ml)
  6. dry with materialCombined extracts were dried (Na2SO4)
  7. customevaporated in vacuo
  8. customto give an oil which
  9. filtrationThe mixture was filtered
  10. customthe filtrate evaporated in vacuo