反应 #94743

反应方程式

2-(3,4-dimethoxyphenyl)-1-nitroethane

1-iodo-5-phenyl-3-pentanone

→

crude oil

收率 113.2%

1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone

收率 113.2%

溶剂

tetrahydrofuran

tetrahydrofuran

反应条件

后处理

1. 1
   workup.STIRRINGThe mixture was stirred at room temperature for 30 min, at 50° C. for 3 hr
2. 2
   workup.STIRRINGto stir at room temperature overnight
3. 3
   其他Solvent was removed in vacuo
4. 4
   萃取extracted twice with water
5. 5
   干燥The organic layer was dried over anh Mg SO4
6. 6
   浓缩concentrated at reduced pressure

实验过程

To a solution of 36 g (0.17 mole) of 2-(3,4-dimethoxyphenyl)-1-nitroethane in 300 mL of dry tetrahydrofuran was added 71 g (0.17 mole) of 40% Triton B. The solution was stirred at room temperature for 10 min. 55.3 g (0.19 mole) of 1-iodo-5-phenyl-3-pentanone in a minimum amount of dry tetrahydrofuran was added dropwise. The mixture was stirred at room temperature for 30 min, at 50° C. for 3 hr., then allowed to stir at room temperature overnight. Solvent was removed in vacuo and the residue taken up in ether and extracted twice with water. The organic layer was dried over anh Mg SO4, and concentrated at reduced pressure to give 71.5 g of crude oil. This crude material was passed through HPLC to give 46.4 g. of purified material.

来源