تفاعل #167718

معادلة التفاعل

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

المردود 52.0%

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe suspension was warmed up naturally and
2. 2
   workup.DISSOLUTIONto dissolve
3. 3
   أخرىthe precipitation
4. 4
   استخلاصThe combined organic layers from extraction
5. 5
   أخرىdried
6. 6
   تركيزconcentrated

الإجراء التجريبي

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).

المصدر