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phosphoric acid

1-isobutylcyclohexanol

phosphoric acid

1-isobutylcyclohexanol

→

1-isobutylcyclohex-1-ene

용매

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후처리

1. 1
   workup.DISTILLATIONWhile 1-isobutylcyclohex-1-ene and water distilled (boiling point 60° C.)
2. 2
   workup.ADDITIONAt the end of the addition
3. 3
   온도heated further (vacuum from 170 to 40 mbar)
4. 4
   기타The distillate was decanted
5. 5
   추출the water phase extracted with pentane (100 ml)
6. 6
   건조phases were dried (MgSO4)
7. 7
   기타the solvent evaporated

실험 절차

In a flask equipped with a Vigreux-distillation apparatus, crude 1-isobutylcyclohexanol (200 g, 1.28 mol) was treated with phosphoric acid (100 g) and heated at 145° C. under vacuum (170 mbar). While 1-isobutylcyclohex-1-ene and water distilled (boiling point 60° C.), a second fraction of 1-isobutylcyclohexanol (492 g, 3.15 mol) was added dropwise in the reaction flask. At the end of the addition, the thick reaction mixture was diluted with paraffin oil (100 ml) and additional phosphoric acid (50 g) and heated further (vacuum from 170 to 40 mbar). The distillate was decanted and the water phase extracted with pentane (100 ml). The combined org. phases were dried (MgSO4) and the solvent evaporated to give 1-isobutylcyclohex-1-ene (448 g, 78%).

출처