Sodium Acetate → HCID 54311389, compound

Participants

Reaction Steps

A mixture of 27.5 g of ethyl β-ethyl-β-iminopropionate hydrochloride, 30 g of 2,6 -dichloro-4-methoxycarbonylphenylhydrazine [Intermediate (h) as in Method (a) in Syntheses Example 1-(1)] and 11.5 g of anhydrous sodium acetate in 100 ml of methanol as stirred at room temperature for 2 hours. A solution containing 7 g of metallic sodium dissolved in 70 ml of methanol was added dropwise to the mixture, and the mixture was further stirred at room temperature for 2 hours. After adding 60 ml of acetic acid, the reaction mixture was poured into 1 liter of water. The crystals formed were collected and recrystallized from acetonitrile to obtain 21 g of 1-(2,6 -dichloro-4-methoxycarbonylphenyl)-3-amino-5-pyrazolone having a melting point of 225°-229°C.

Provenance & Evidence