تفاعل #155972

معادلة التفاعل

1,4-Dioxa-8-azaspiro[4.5]decane

2,5-dichloropyrimidine

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title compound

8-(5-Chloropyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane

المذيبات

N,N-dimethylformamide

1,4-dioxane

triethylamine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture is heated
2. 2
   درجة الحرارةAfter cooling to room temperature
3. 3
   تركيزthe solution is concentrated
4. 4
   أخرىpartitioned between dichloromethane (100 mL) and water (100 mL)
5. 5
   استخلاصThe aqueous layer is extracted with dichloromethane (100 mL)
6. 6
   غسيلwashed with water (2×100 mL)
7. 7
   تجفيفdried over Na2SO4
8. 8
   ترشيحfiltered
9. 9
   تركيزconcentrated

الإجراء التجريبي

1,4-Dioxa-8-azaspiro[4.5]decane (2.39 g) is combined with 2,5-dichloropyrimidine (2.44 g) in N,N-dimethylformamide (50 mL), 1,4-dioxane (75 mL) and triethylamine (6.7 mL) in a glass pressure reaction vessel. The mixture is heated with stirring at 120° C. for 16 h. After cooling to room temperature, the solution is concentrated and partitioned between dichloromethane (100 mL) and water (100 mL). The aqueous layer is extracted with dichloromethane (100 mL). The dichloromethane layers are combined, washed with water (2×100 mL), dried over Na2SO4, filtered and concentrated to yield the title compound.

المصدر