反応 #706492

反応方程式

compound

4-Methoxycarbonyl-3,5-heptanedione

2,6-dichloro-4-trifluoromethylphenyl hydrazine

→

desired product

収率 43.0%

Methyl 1-(2,6-dichloro-4-trifluoromethylphenyl)-3,5-diethylpyrazole-4-carboxylate

収率 43.0%

溶媒

ethanol

反応条件

後処理

1. 1
   温度at reflux for 8 hours
2. 2
   その他The ethanol was removed by evaporation
3. 3
   その他the residues were partitioned between ethyl acetate and dilute hydrogen chloride
4. 4
   その他The organic extracts were dried
5. 5
   その他evaporated

実験手順

A solution of 7.5 g (40 mmol) of the compound of step A and 11.85 g (48 mmol) of 2,6-dichloro-4-trifluoromethylphenyl hydrazine in 50 mL of ethanol was heated at reflux for 8 hours. The ethanol was removed by evaporation and the residues were partitioned between ethyl acetate and dilute hydrogen chloride. The organic extracts were dried and evaporated to give the desired product in 43% yield as a maroon oil. 1H-NMR (CDCl3) δ1.08 (3H, t, J=7), 1.24 (3H, t, J=7), 2.22 (2H, q, J=7), 2.94 (2H, q, J=7), 3.86 (3H, s), 7.46 (2H, s).

出典