تفاعل #56664

معادلة التفاعل

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

المذيبات

THF

THF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto maintain the mixture at the reflux temperature
2. 2
   درجة الحرارةthe mixture is refluxed for 2.5 hours
3. 3
   درجة الحرارةat reflux temperature for 1 hour
4. 4
   استخلاصextracted with ethyl acetate
5. 5
   أخرىThe organic phase is dried
6. 6
   ترشيحafter filtration
7. 7
   أخرىthe solvent is evaporated off under reduced pressure
8. 8
   أخرىThe residue is crystallized in ethyl acetate
9. 9
   أخرىThe product of the title is obtained in the form of a white solid

الإجراء التجريبي

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.

المصدر