반응 #696700
ord-26d728dca65e4327955dcc14f90f46d3
반응 방정식
반응 조건
후처리
- 1기타To a 200-ml three-necked round flask (equipped with a stirrer tip
- 2workup.ADDITIONAfter the dropwise addition
- 3기타was elevated to 50° C.
- 4기타reaction for further 3.5 hours
- 5기타After the reaction
- 6온도the mixture was cooled
- 7농축Then, the reaction mixture was concentrated under reduced pressure
- 8추출extracted with 50 ml of water and 50 ml of ether
- 9기타The organic phase was separated
- 10추출the aqueous phase was extracted twice with 50 ml of ether
- 11세척The combined organic phases were washed with 100 ml of a saturated saline solution
- 12건조dried over anhydrous Na2SO4
- 13workup.DISTILLATIONThen, the solvent was distilled off under reduced pressure
실험 절차
To a 200-ml three-necked round flask (equipped with a stirrer tip, a Dimroth condenser, a dropping funnel and a thermometer) were introduced 0.85 g (22.6 mmol) of sodium boron hydride and 28 ml of ethanol, and then in a nitrogen atmosphere at room temperature, a solution of 10.6 g (45.1 mmol) of 2-ethyl-4-phenyl-1-indanone in 20 ml of ethanol was dropwise added. After the dropwise addition was completed, the temperature was elevated to 50° C. to perform reaction for further 3.5 hours. After the reaction, the mixture was cooled, and acetone was dropwise added to decompose the unreacted sodium boron hydride. Then, the reaction mixture was concentrated under reduced pressure and extracted with 50 ml of water and 50 ml of ether. The organic phase was separated, and the aqueous phase was extracted twice with 50 ml of ether. The combined organic phases were washed with 100 ml of a saturated saline solution and dried over anhydrous Na2SO4. Then, the solvent was distilled off under reduced pressure to obtain 10.67 g of the aimed product (a mixture of two isomers) as a viscous, light yellow liquid (yield: 99%). The properties of the product thus obtained are described below.