反应 #65181

反应方程式

Phenylmalonic acid

thionyl chloride

cyclohexyl alcohol

→

cyclohexyl hydrogen phenylmalonate

溶剂

ether

反应条件

后处理

1. 1
   温度The mixture was heated at 40°-50° C. for 3 hours
2. 2
   workup.DISTILLATIONThe clear solution was distilled under vacuum
3. 3
   workup.DISSOLUTIONThe oily residue was redissolved in dry ether (40 mL)
4. 4
   温度refluxed for 2 hours
5. 5
   其他to give an oily product which
6. 6
   其他crystallized
7. 7
   其他Recrystallization
8. 8
   其他was carried out from a benzenepetroleum ether (40°-60°) mixture
9. 9
   其他to give a white crystalline product

实验过程

Phenylmalonic acid (13.5 g, 0.07 mol) in dry ether (40 mL) was treated with thionyl chloride (8.92 g, 5.4 mL, 0.07 mol) and one drop of N,N-dimethylformamide. The mixture was heated at 40°-50° C. for 3 hours. The clear solution was distilled under vacuum. The oily residue was redissolved in dry ether (40 mL), the solution was treated with cyclohexyl alcohol (0.075 mol, 7.9 mL) and refluxed for 2 hours. The mixture was worked up as before to give an oily product which crystallized on standing. Recrystallization was carried out from a benzenepetroleum ether (40°-60°) mixture to give a white crystalline product.

来源