反应 #2069937

反应方程式

ethyl chlorocarbonate

3-amino-4,6-dihydro-1H-pyrrolo[3,4-c]pyrazole-5-carboxylic acid tert-butyl ester

DIEA

→

title compound

收率 72.0%

3-Amino-4,6-dihydro-pyrrolo[3,4-c]pyrazole-1,5-dicarboxylic acid 5-tert-butyl ester 1-ethyl ester

收率 72.0%

溶剂

THF

THF

反应条件

后处理

1. 1
   其他to reach r.t.
2. 2
   其他The obtained mixture was evaporated to dryness under vacuum
3. 3
   萃取The resulting residue was extracted with AcOEt and water
4. 4
   其他The organic phase was separated
5. 5
   干燥dried over sodium sulfate
6. 6
   其他evaporated to dryness
7. 7
   其他The mixture was purified by flash-chromatography (eluent: ethyl acetate/cyclohexane 4/6 to 7/3)

实验过程

A solution of ethyl chlorocarbonate (8.9 ml, 93 mmol) in THF (250 ml) was added slowly to a mixture of 3-amino-4,6-dihydro-1H-pyrrolo[3,4-c]pyrazole-5-carboxylic acid tert-butyl ester (20 g, 89 mmol) and DIEA (92 ml, 528 mmol) in THF (500 ml) at 0-5° C. The reaction was kept at the same temperature for two hours then allowed to reach r.t. and stirred overnight. The obtained mixture was evaporated to dryness under vacuum. The resulting residue was extracted with AcOEt and water. The organic phase was separated, dried over sodium sulfate and evaporated to dryness. The mixture was purified by flash-chromatography (eluent: ethyl acetate/cyclohexane 4/6 to 7/3) to give 19 g (72% yield) of the title compound as a white solid.

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