反应 #792179

反应方程式

1,1,1-Trifluoroacetone

3-chloro-2(1H)-pyridinone hydrazone

(3-chloro-pyridin-2-yl)-hydrazine

→

product

收率 66.0%

3-chloro-2(1H)-pyridinone (2,2,2-trifluoro-1-methylethylidene)hydrazone

收率 66.0%

反应条件

后处理

1. 1
   workup.ADDITIONAfter the addition
2. 2
   其他The solvent was removed under reduced pressure
3. 3
   其他the mixture partitioned between ethyl acetate (100 mL) and saturated aqueous sodium carbonate solution (100 mL)
4. 4
   其他The organic layer was dried
5. 5
   其他evaporated
6. 6
   其他Chromatography on silica gel (eluted with ethyl acetate) gave

实验过程

1,1,1-Trifluoroacetone (7.80 g, 69.6 mmol) was added to 3-chloro-2(1H)-pyridinone hydrazone (alternatively named (3-chloro-pyridin-2-yl)-hydrazine) (10 g, 69.7 mmol) at 20-25° C. After the addition was complete, the mixture was stirred for about 10 minutes. The solvent was removed under reduced pressure and the mixture partitioned between ethyl acetate (100 mL) and saturated aqueous sodium carbonate solution (100 mL). The organic layer was dried and evaporated. Chromatography on silica gel (eluted with ethyl acetate) gave the product as an off-white solid (11 g, 66% yield), m.p. 64-64.5° C. (after crystallization from ethyl acetate/hexanes).

来源