반응 #1142873

반응 방정식

compound

1-(2,2-Diethoxyethyl)-3-(pyridin-3-yl)-1H-pyrazole-5-amine

1-bromo-2-chloro-4-methyl-5-nitrobenzene

→

N-(2-Chloro-4-methyl-5-nitrophenyl)-1-(2,2-diethoxyethyl)-3-(pyridin-3-yl)-1H-pyrazole-5-amine

반응 조건

후처리

1. 1
   기타gave, after 2 h
2. 2
   온도of heating
3. 3
   온도under reflux
4. 4
   기타a crude product which was purified by double chromatography on a Biotage system (in each case 50 g Snap column
5. 5
   온도mobile phase gradient hexane/ethyl acetate, from 20% ethyl acetate increasing rapidly to 100% ethyl acetate, then ethyl acetate/methanol, increasing slowly to 100% methanol)

실험 절차

Analogously to Example 13A/Step 1, from two reactions (273 mg and 1.58 g; 6.72 mmol in total) of the compound of Example 4A and 250 mg and 1.45 g (7.4 mmol in total) of 1-bromo-2-chloro-4-methyl-5-nitrobenzene gave, after 2 h of heating under reflux, a crude product which was purified by double chromatography on a Biotage system (in each case 50 g Snap column; mobile phase gradient hexane/ethyl acetate, from 20% ethyl acetate increasing rapidly to 100% ethyl acetate, then ethyl acetate/methanol, increasing slowly to 100% methanol). This gave 1.96 g (69% of theory) of the title compound.

출처