반응 #160659

반응 방정식

iodine

phosphorous acid

4-Bromobenzhydrol

→

4-Bromodiphenylmethane

수율 61.0%

용매

acetic acid

반응 조건

후처리

1. 1
   온도cooled
2. 2
   추출the reaction mixture was extracted with hexane (200 ml) 5 times
3. 3
   세척The combined organic layer was washed with 10 wt. % KOH solution and 200 ml of a saturated ammonium chloride solution
4. 4
   세척further washed with a saturated Na2SO3 solution twice
5. 5
   기타The solvent was evaporated
6. 6
   기타the result product was dried under vacuum
7. 7
   기타to provide a yield of 61% (276 mmol)

실험 절차

4-Bromodiphenylmethane was prepared as shown in Scheme 3. 4-Bromobenzhydrol in a 3-neck flask equipped with a reflux condenser and a thermometer was mixed with 500 ml of acetic acid, 113 g (445 mmol) of iodine and 226 ml, 50 wt. % of phosphorous acid (2.2 mol). The reaction mixture was heated at 80° C. for 24 hours and then cooled. 700 ml of ice-water was added to the reaction mixture and the reaction mixture was extracted with hexane (200 ml) 5 times. The combined organic layer was washed with 10 wt. % KOH solution and 200 ml of a saturated ammonium chloride solution and then further washed with a saturated Na2SO3 solution twice. The solvent was evaporated and the result product was dried under vacuum to provide a yield of 61% (276 mmol). BP: 103° C. (5*10−2 mbar)

출처