反应 #61692

反应方程式

sodium

methyl ester

methyl 9-hydroxyfluorene-9-carboxylate

tropenol

sodium

water

→

tropenol 9-hydroxyfluorene-9-carboxylate

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度After cooling
2. 2
   其他the solution is evaporated to dryness
3. 3
   萃取the residue is extracted with dichloromethane/water
4. 4
   洗涤The organic phase is washed with water
5. 5
   干燥dried over magnesium sulfate (MgSO4)
6. 6
   workup.DISTILLATIONthe solvent is distilled off
7. 7
   其他The product is purified by recrystallization from diethyl ether

实验过程

13.4 g (0.056 mol) of methyl ester 3a, 11.65 g (0.084 mol) of tropenol, and 0.3 g of sodium are heated as a melt at 75 mbar for 4 hours over a bath of boiling water with occasional agitation. After cooling, the sodium residues are dissolved with acetonitrile, the solution is evaporated to dryness, and the residue is extracted with dichloromethane/water. The organic phase is washed with water, dried over magnesium sulfate (MgSO4), and the solvent is distilled off. The product is purified by recrystallization from diethyl ether. Yield: 11.40 g of white crystals (29% of theoretical yield).

来源