反応 #792179

反応方程式

1,1,1-Trifluoroacetone

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

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

→

product

収率 66.0%

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

収率 66.0%

反応条件

後処理

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

実験手順

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).

出典