HRID991493
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureat reflux for 1 h
- temperaturecooled
- customevaporated in vacuo
- customResidue was partitioned between water (1 L) and dichloromethane (4×200 ml)
- dry with materialCombined extracts were dried (Na2SO4)
- customevaporated in vacuo
- customto give an oil which
- filtrationThe mixture was filtered
- customthe filtrate evaporated in vacuo