تفاعل #2461964

معادلة التفاعل

Oxalyl chloride

6-chloro-3-oxo-2,3-dihydro-pyridazine-4-carboxylic acid

DMF

→

6-Chloro-3-oxo-2,3-dihydro-pyridazine-4-carboxylic acid 4-chloro-benzyl amide

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   أخرىAfterwards, it was evaporated to dryness
2. 2
   workup.DISSOLUTIONthe residue dissolved in 450 ml THF
3. 3
   workup.ADDITION13.8 g potassium carbonate and a solution of 7.2 g 4-chloro-benzyl amide in THF were added
4. 4
   workup.DISTILLATIONThe solvent was distilled off after 2 h
5. 5
   workup.STIRRINGof stirring at room temperature
6. 6
   تجفيفdried over phosphorous pentoxide in an desiccator

الإجراء التجريبي

Oxalyl chloride was added to a solution a 8.73 g of 6-chloro-3-oxo-2,3-dihydro-pyridazine-4-carboxylic acid and 1 ml DMF in 250 ml THF at 5-10° C. and the mixture was stirred at room temperature for 2 h. Afterwards, it was evaporated to dryness, the residue dissolved in 450 ml THF and 13.8 g potassium carbonate and a solution of 7.2 g 4-chloro-benzyl amide in THF were added. The solvent was distilled off after 2 h of stirring at room temperature, the residue suspended in 100 ml water and a pH of 6.4 was adjusted. The obtained precipitate was sucked off, suspended again in 50 ml water and the pH is adjusted to 3. Afterwards, the precipitate was sucked off and dried over phosphorous pentoxide in an desiccator.

المصدر