반응 #792179

반응 방정식

1,1,1-Trifluoroacetone

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

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

→

product

수율 66.0%

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

수율 66.0%

반응 조건

후처리

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

실험 절차

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).

출처