تفاعل #1275150

معادلة التفاعل

4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydro-isoxazole-3-yl]-2-methyl-N-(5-pyrimidinyl)benzoic acid amide

triethylamine

methyl chloroformate

→

aimed product

المردود 50.1%

Methyl N-[4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydro-isoxazole-3-yl]-2-methylbenzoyl]-N-(5-pyrimidinyl)carbamate

المردود 50.1%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter the completion of the reaction
2. 2
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure, 10 mL of ethyl acetate
3. 3
   workup.ADDITIONwas added
4. 4
   ترشيحinsoluble material was filtered off
5. 5
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
6. 6
   أخرىthe residue was purified with silica gel column chromatography that

الإجراء التجريبي

In a solution of 0.25 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydro-isoxazole-3-yl]-2-methyl-N-(5-pyrimidinyl)benzoic acid amide synthesized in Step 1 of Synthetic Example 14, 0.15 g of triethylamine and a catalytic amount of 4-(dimethylamino)pyridine in 4 mL of tetrahydrofuran, 0.15 g of methyl chloroformate was added, and stirred at room temperature for 16 hours. After the completion of the reaction, the solvent was distilled off under reduced pressure, 10 mL of ethyl acetate was added and insoluble material was filtered off. The solvent was distilled off under reduced pressure and the residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (1:1) to obtain 0.14 g of the aimed product as white crystal.

المصدر