反应详情

温度

5 °C

Phosphorusoxychloride (53.7 g, 350 mmol) is slowly added to DMF (60 mL) stirred at 5° C. Upon complete addition, the clear solution is stirred for further 30 min at 5° C. before 5-methyl-2-hexanone (20 g, 175 mmol) is added dropwise. The yellow solution is stirred for 30 min at 0° C., then for 90 min at rt. The mixture becomes warm (40° C.) and a thick suspension forms. The mixture is cooled to 25° C. and stirring is continued for 1 h before it is poured into an aq. solution of NaOAc (80 g)/ice mixture. The mixture is extracted twice with diethyl ether. The organic extracts are washed with water, combined, dried over MgSO4, filtered and evaporated to give crude 3-chloro-2-isobutyl-but-2-enal (35.4 g) as a yellow oil, LC-MS: tR=0.97 min.

1. additionUpon complete addition
2. additionis added dropwise
3. stirringThe yellow solution is stirred for 30 min at 0° C.
4. temperatureThe mixture becomes warm (40° C.)
5. temperatureThe mixture is cooled to 25° C.
6. stirringstirring
7. waitis continued for 1 h before it
8. extractionThe mixture is extracted twice with diethyl ether
9. washThe organic extracts are washed with water
10. dry with materialdried over MgSO4
11. filtrationfiltered
12. customevaporated