반응 #44203

반응 방정식

HCl

Ethyl acetimidate HCl salt

Et3N

4-(4-bromo-2-fluorophenylamino)-5-fluoro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid hydrazide

→

desired product

4-(4-bromo-2-fluorophenylamino)-5-fluoro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid N′-(1-imino-ethyl)-hydrazide

용매

THF

DMF

반응 조건

후처리

1. 1
   기타at 0° C
2. 2
   workup.ADDITION17 hours at room temperature, the reaction mixture was poured onto water
3. 3
   추출extracted with ethyl acetate
4. 4
   건조The combined organic extracts were dried (MgSO4)
5. 5
   농축concentrated under reduced pressure

실험 절차

Ethyl acetimidate HCl salt (40 mg, 0.32 mmol) and Et3N (0.049 mL, 0.35 mmol) were added to a stirred suspension of 4-(4-bromo-2-fluorophenylamino)-5-fluoro-1-methyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid hydrazide (0.10 g, 0.27 mmol) in 2:1 THF:DMF (3 mL) at 0° C. After 1.5 hours at 0° C. and 17 hours at room temperature, the reaction mixture was poured onto water, neutralized with dilute aqueous HCl and extracted with ethyl acetate. The combined organic extracts were dried (MgSO4) and concentrated under reduced pressure. Trituration with methylene chloride gave the desired product.

출처