반응 #56664

반응 방정식

NH4Cl

1,4-cyclohexandione monoethyleneacetal

2-(4-bromophenyl)-4,4-dimethyl-4,5-dihydro-1,3-oxazole

→

8-[4-(4,4-Dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenyl]-1,4-dioxaspiro[4,5]decan-8-ol

용매

THF

THF

반응 조건

후처리

1. 1
   온도to maintain the mixture at the reflux temperature
2. 2
   온도the mixture is refluxed for 2.5 hours
3. 3
   온도at reflux temperature for 1 hour
4. 4
   추출extracted with ethyl acetate
5. 5
   기타The organic phase is dried
6. 6
   여과after filtration
7. 7
   기타the solvent is evaporated off under reduced pressure
8. 8
   기타The residue is crystallized in ethyl acetate
9. 9
   기타The product of the title is obtained in the form of a white solid

실험 절차

A solution of 8 g of 2-(4-bromophenyl)-4,4-dimethyl-4,5-dihydro-1,3-oxazole (31.5 mmol) in 15 ml of anhydrous THF is poured dropwise onto 956 mg of Mg (39.3 mmol) in such a way as to maintain the mixture at the reflux temperature and the mixture is refluxed for 2.5 hours. The mixture is cooled to room temperature and a solution of 5.41 g of 1,4-cyclohexandione monoethyleneacetal (34.65 mmol) in 20 ml of anhydrous THF is added to it dropwise. The mixture is stirred at room temperature for 1.5 hours and then at reflux temperature for 1 hour. The mixture is poured into 500 ml of a 10% NH4Cl solution and extracted with ethyl acetate. The organic phase is dried and, after filtration, the solvent is evaporated off under reduced pressure. The residue is crystallized in ethyl acetate. The product of the title is obtained in the form of a white solid.

출처