반응 #94743

반응 방정식

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

1-iodo-5-phenyl-3-pentanone

→

crude oil

수율 113.2%

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

수율 113.2%

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

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
   기타Solvent was removed in vacuo
4. 4
   추출extracted twice with water
5. 5
   건조The organic layer was dried over anh Mg SO4
6. 6
   농축concentrated at reduced pressure

실험 절차

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.

출처