반응 #64733

반응 방정식

sodium hydride

tertiary-butyl(diethoxymethyl)-phosphine oxide

iso-butyl bromide

→

tertiary-butyl-(iso-butyl)(diethoxymethyl)phosphine oxide

용매

tetrahydrofuran

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.DISSOLUTIONthe solid dissolves
2. 2
   기타To the clear solution obtained
3. 3
   workup.ADDITIONAfter the addition
4. 4
   온도the reaction mixture is heated
5. 5
   온도under reflux for 15 hours
6. 6
   세척washed with 20 ml of water
7. 7
   기타The organic extracts are dried
8. 8
   기타evaporated under reduced pressure
9. 9
   기타The crude product is purified by chromatography on silica

실험 절차

Dry sodium hydride (0.42 g) is suspended in 50 ml of dry tetrahydrofuran under an argon atmosphere. To this stirred suspension is added 3.6 g (0.017 mol) of tertiary-butyl(diethoxymethyl)-phosphine oxide dissolved in 25 ml of dry tetrahydrofuran, at room temperature. Stirring is continued for 10 minutes at room temperature, during which time the solid dissolves and a gas is evolved. To the clear solution obtained is added a solution of 2.4 g (0.017 mol) of iso-butyl bromide in 25 ml of dry tetrahydrofuran. After the addition is complete, the reaction mixture is heated under reflux for 15 hours, then allowed to cool at room temperature and washed with 20 ml of water. The organic extracts are dried and evaporated under reduced pressure. The crude product is purified by chromatography on silica using ethyl acetate as eluent to give tertiary-butyl-(iso-butyl)(diethoxymethyl)phosphine oxide as a colourless oil.

출처