تفاعل #61068

معادلة التفاعل

water

4-Chloro-butyryl chloride

3-aminopyrazole

K2HPO4

→

title compound

المردود 34.0%

4-Chloro-N-[1-(4-chlorobutanoyl)-1H-pyrazol-3-yl]butanamide

المردود 34.0%

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe reaction mixture was stirred for 24 hr
2. 2
   أخرىthe phases were separated
3. 3
   استخلاصThe aqueous layer was extracted with EtOAc (2×20 mL)
4. 4
   تجفيفthe combined organic extracts were dried over anh. Na2SO4
5. 5
   ترشيحThe solids were filtered
6. 6
   أخرىthe solvent evaporated
7. 7
   أخرىThe crude product was purified by flash chromatography (silica gel, cHex/EtOAc 7:3)

الإجراء التجريبي

To a solution of 3-aminopyrazole (300 mg, 3.61 mmol) in anh. CH2Cl2 (6 mL), at r.t., under N2, was added K2HPO4 (1.26 g, 2 eq) and the reaction mixture was stirred at r.t. for 15 min. 4-Chloro-butyryl chloride (406 μL, 3.6 mmol) was then added and the reaction mixture was stirred for 24 hr. It was then poured into water and the phases were separated. The aqueous layer was extracted with EtOAc (2×20 mL) and the combined organic extracts were dried over anh. Na2SO4. The solids were filtered and the solvent evaporated. The crude product was purified by flash chromatography (silica gel, cHex/EtOAc 7:3) to give the title compound as a white solid (354 mg, 34%)

المصدر