반응 #167718

반응 방정식

Water

5-bromo-N3-(2-chloro-3,6-difluorobenzyl)pyrazine-2,3-diamine

N,N-diethylisopropylamine

ethyl glyoxylate

→

ethyl ({5-bromo-3-[(2-chloro-3,6-difluorobenzyl)amino]pyrazin-2-yl}amino)(oxo)acetate

수율 52.0%

용매

CH2Cl2

반응 조건

후처리

1. 1
   온도The suspension was warmed up naturally and
2. 2
   workup.DISSOLUTIONto dissolve
3. 3
   기타the precipitation
4. 4
   추출The combined organic layers from extraction
5. 5
   기타dried
6. 6
   농축concentrated

실험 절차

To a stirred solution of 5-bromo-N3-(2-chloro-3,6-difluorobenzyl)pyrazine-2,3-diamine (5.15 mmol, 1.8 g) and N,N-diethylisopropylamine (9.30 mmol, 2 mL) in CH2Cl2 (20 mL) was added ethyl glyoxylate (5.41 mmol, 0.74 g) at 0° C. The suspension was warmed up naturally and stirred overnight. Water was added to dissolve the precipitation. The combined organic layers from extraction were combined, dried, concentrated, and then subjected to a silica gel column chromatography by using CH2Cl2/MeOH (9:1) as eluents, furnishing ethyl ({5-bromo-3-[(2-chloro-3,6-difluorobenzyl)amino]pyrazin-2-yl}amino)(oxo)acetate in 52% yield (1.20 g).

출처