反应详情

温度

138 °C

To a stirred suspension of 1-methylamino-2,4-dinitrobenzene (1.00 g, 5.07 mmol) in xylenes (10 mL) was added methyl-5-chloro-5-oxo-valerate (3.50 mL, 25.28 mmol, 5.0 equiv.) at 20° C. The reaction mixture was then heated to reflux, approximately 138° C. Reaction progress was monitored periodically by HPLC Method A. The reaction was complete after stirring for approximately 24 hours at 138° C. The reaction mixture was cooled to 0° C. and hexanes was added (10 mL) to crystallize the product. The resultant slurry was stirred for approximately 1 hour at −10° C. to 0° C. and then filtered. The wet cake was dried at 60° C. under vacuum/N2 sweep overnight to give 1.30 g (79% yield) as an off-while solid.

1. temperatureThe reaction mixture was then heated
2. customReaction progress
3. temperatureThe reaction mixture was cooled to 0° C.
4. customto crystallize the product
5. stirringThe resultant slurry was stirred for approximately 1 hour at −10° C. to 0° C.
6. filtrationfiltered
7. dry with materialThe wet cake was dried at 60° C. under vacuum/N2
8. waitsweep overnight
9. customto give 1.30 g (79% yield) as an off-while solid