반응 #42161

반응 방정식

sodium-tert-butoxide

chlorobenzene

propiophenone

tetrahydrofuran

→

1,2-diphenyl-1-propanone

수율 77.4%

용매

water

반응 조건

후처리

1. 1
   기타A 30-ml four-necked flask was equipped with a stirrer
2. 2
   workup.ADDITIONadded into the flask
3. 3
   기타The flask was purged with argon
4. 4
   workup.STIRRINGby stirring at 22° C. for 30 minutes
5. 5
   workup.STIRRINGby stirring at 22° C. for 30 minutes
6. 6
   workup.STIRRINGby stirring at 70° C. for 6 hours
7. 7
   workup.ADDITIONwas added
8. 8
   기타followed by separation
9. 9
   기타The organic phase was purified by column chromatography

실험 절차

A 30-ml four-necked flask was equipped with a stirrer, a thermometer and a reflux condenser. 0.022 g (0.1 mmol) of palladium (II) acetate, 0.721 g (7.5 mmol) of sodium-tert-butoxide and 5 ml of tetrahydrofuran were weighed in the flask, followed by stirring. Further, 0.052 g (0.1 mmol) of tri-tert-butylphosphonium tetraphenylborate obtained in Example A-1 was weighed in air and added into the flask. The flask was purged with argon, followed by stirring at 22° C. for 30 minutes. 0.563 g (5 mmol) of chlorobenzene was added, followed by stirring at 22° C. for 30 minutes. 0.738 g (5.5 mmol) of propiophenone was added, followed by stirring at 70° C. for 6 hours. After the completion of the reaction, 2.5 ml of water was added, followed by separation. The organic phase was purified by column chromatography to afford 0.814 g of 1,2-diphenyl-1-propanone (yield: 77 mol % based on chlorobenzene). The identification of the product was made by mass spectroscopy, 1H-NMR and 13C-NMR.

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