تفاعل #68483

معادلة التفاعل

tert-butyl (6-ethynyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylcarbamate

triethylamine

nitroethane

phenyl isocyanate

→

product

tert-butyl(6-(3-methylisoxazol-5-yl)-[1,2,4]-triazolo[4,3-b]pyridazin-3-yl)methylcarbamate

المذيبات

benzene

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGThe mixture was stirred at 50° C. for six hours
2. 2
   أخرىat room temperature
3. 3
   أخرىovernight
4. 4
   درجة الحرارةThe mixture was cooled to room temperature
5. 5
   ترشيحfiltered
6. 6
   غسيلthe resulting brown precipitate was washed with additional benzene
7. 7
   تركيزThe filtrate was concentrated

الإجراء التجريبي

To a solution of nitroethane (1.02 ml, 14.3 mmol) in benzene (50 mL) was added phenyl isocyanate (3.12 ml, 28.5 mmol). The mixture was stirred at 50° C. for twenty minutes followed by the addition of tert-butyl (6-ethynyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylcarbamate (3.00 g, 11.0 mmol) and triethylamine (0.0765 ml, 0.549 mmol). The mixture was stirred at 50° C. for six hours then at room temperature overnight. The mixture was cooled to room temperature, filtered and the resulting brown precipitate was washed with additional benzene. The filtrate was concentrated to yield the product as a black solid. MS m/z=331.1 [M+1]+. Calc'd for C15H18N6O3: 330.1.

المصدر