反応 #48591

反応方程式

Bis(2-chloroethyl)methylamine hydrochloride

4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide

diisopropyethylamine

→

solid

収率 19.8%

4-(4-Methyl-piperazin-1-yl)-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide

収率 19.8%

溶媒

DMF

反応条件

後処理

1. 1
   その他The DMF was removed under vacuum
2. 2
   その他purified by flash column chromatography
3. 3
   洗浄eluting with dichloromethane/methanol/acetic acid/water (90:18:3:2)
4. 4
   workup.ADDITIONProduct containing fractions
5. 5
   その他evaporated
6. 6
   workup.ADDITIONtreated with HCl in ethyl acetate
7. 7
   その他re-evaporated with toluene (2×20 ml)

実験手順

Bis(2-chloroethyl)methylamine hydrochloride (97 mg; 0.5 mmol) was added to a stirred solution of 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (100 mg; 0.45 mmol), tetrabutylammonium iodide (20 mg; 0.045 mmol) and diisopropyethylamine (200 ul) 1.13 mmol) in DMF (5 ml), and the resulting mixture was heated at 200° C. (100 W) for 30 minutes in a CEM Discover™ microwave synthesiser. The DMF was removed under vacuum, then purified by flash column chromatography, eluting with dichloromethane/methanol/acetic acid/water (90:18:3:2). Product containing fractions were combined and evaporated, treated with HCl in ethyl acetate and then re-evaporated with toluene (2×20 ml) to give an off white solid (27 mg). (LC/MS: Rt 1.64, [M+H]+ 378).

出典