تفاعل #2069937

معادلة التفاعل

ethyl chlorocarbonate

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

DIEA

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title compound

المردود 72.0%

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

المردود 72.0%

المذيبات

THF

THF

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر