반응 #68489

반응 방정식

1-(6-chloropyridazin-3-yl)hydrazine

2-(quinolin-6-yl)acetic acid

HCl

→

6-((6-Chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)quinoline

용매

Na2CO3

반응 조건

후처리

1. 1
   온도was heated in a microwave (Personal Chemistry) at 180° C.
2. 2
   기타15 min
3. 3
   기타The mixture was quenched with a solution of NaOH (1.2 g, 5 mL) slowly until the suspension
4. 4
   여과The mixture was filtered
5. 5
   세척washed with H2O (2×5 mL)
6. 6
   기타A brown solid was obtained (2.2 g)
7. 7
   온도heated at 50° C. for 30 min
8. 8
   온도The blue mixture was cooled to room temperature
9. 9
   여과filtered
10. 10
    세척The black solid was washed with H2O
11. 11
    기타to give the product

실험 절차

A mixture of 1-(6-chloropyridazin-3-yl)hydrazine (1.67 g, 12 mmol), 2-(quinolin-6-yl)acetic acid (1.65 g, 8.8 mmol), and HCl (2000 μl, 24 mmol) was heated in an oil bath at 110° C. for 20 min before it was heated in a microwave (Personal Chemistry) at 180° C.& 15 min. The mixture was quenched with a solution of NaOH (1.2 g, 5 mL) slowly until the suspension is neutral in pH. The mixture was filtered and washed with H2O (2×5 mL). A brown solid was obtained (2.2 g). The solid was treated with aqueous Na2CO3 (3 g, 20 mL, pH ˜11) and heated at 50° C. for 30 min. The blue mixture was cooled to room temperature, and filtered. The black solid was washed with H2O and lyophilized to give the product.

출처