反応 #61068

反応方程式

water

4-Chloro-butyryl chloride

3-aminopyrazole

K2HPO4

→

title compound

収率 34.0%

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

収率 34.0%

溶媒

CH2Cl2

反応条件

後処理

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

実験手順

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%)

出典