反应 #40349
ord-400cdce93deb4c6eb318c93910679f8e
反应方程式
hydrazine
NaNO2
6-amino-4-trifluoromethylquinolin-2(1H)-one
SnCl2.2H2O
→
6-Hydrazino-4-trifluoromethylquinolin-2(1H)-one
反应条件
温度
-1°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.STIRRINGwas stirred at −1° C. for 2 h
- 2其他kept in a refrigerator at −1° C. until it
- 3workup.WAITcan be stored for at least one month without decomposition
实验过程
In a 250 mL r.b. flask a suspension of 6-amino-4-trifluoromethylquinolin-2(1H)-one (structure 8 of Scheme II, where R1=trifluoromethyl) (2.28 g, 10 mmol) in 10 mL conc. HCl was cooled to −1° C. and a solution of NaNO2 (0.40 g, 12 mmol) in water (5 mL) was added dropwise in 20 min. The dark yellow suspension was stirred at −1° C. for 1 h and then a solution of SnCl2.2H2O (5.2 g, 15 mmol) in conc. HCl (10 mL) was added dropwise in 10 min. The light yellow suspension of the hydrazine was stirred at −1° C. for 2 h and then used directly or kept in a refrigerator at −1° C. until it was used (the crude compound can be stored for at least one month without decomposition).