反应详情

温度

90 °C

tert-butyl carbazate, 8.98 g (67.3 mmol) and 3-chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine (11.9 g, 61.1 mmol) were mixed in 1-butanol (245 mL). This mixture was heated till 90° C. and stirred at that temperature for 16 h. The reaction mixture was cooled and water (250 mL) and ethylacetate (250 mL) were added. The biphasic mixture was neutralised with sodium hydrogencarbonate till the pH is 7. Then the organic layer was separated and the water layer was extracted with ethylacetate (250 mL). The combined organic layers were washed once with water (250 mL) and evaporated. The residue was stirred in isopropylether, filtered off and dried under vacuum. Yield: 5.9 g (20.3 mmol; 33%) of the title compound.

1. temperatureThe reaction mixture was cooled
2. customThen the organic layer was separated
3. extractionthe water layer was extracted with ethylacetate (250 mL)
4. washThe combined organic layers were washed once with water (250 mL)
5. customevaporated
6. stirringThe residue was stirred in isopropylether
7. filtrationfiltered off
8. customdried under vacuum