تفاعل #2069938
ord-03c59ebf47294017877d142b189c3983
معادلة التفاعل
المتفاعلات
الكواشف
ظروف التفاعل
المعالجة
- 1تركيزThe reaction mixture was concentrated under vacuum
- 2تركيزconcentrated
- 3أخرىto reach r.t.
- 4workup.STIRRINGstirred overnight
- 5ترشيحThe mixture was filtered
- 6أخرىthe solution evaporated to dryness under vacuum
- 7workup.DISSOLUTIONThe resulting residue was dissolved in DCM
- 8غسيلthe obtained solution was washed with brine
- 9تجفيفdried over sodium sulfate
- 10ترشيحfiltered
- 11أخرىevaporated to dryness
- 12أخرىThe crude product was purified by flash-chromatography (eluent
الإجراء التجريبي
To a solution of 2-naphthalen-2-yl-propionic acid (1.48 g. 7.4 mmol) in DCM (40 ml) and DMF cat., (COCl)2 (0.83 ml, 9.65 mmol) in DCM (10 ml) was added dropwise. The mixture was stirred at r.t. for 30 min. The reaction mixture was concentrated under vacuum, reconstituted twice with toluene and concentrated. A solution of the obtained acyl-chloride in THF (40 ml) was added slowly to a mixture of 3-amino-4,6-dihydro-pyrrolo[3,4-c]pyrazole-1,5-dicarboxylic acid 5-tert-butyl ester 1-ethyl ester (2.0 g, 6.75 mmol) and DIEA (5.8 ml, 33.3 mmol) in THF (40 ml) at 0-5° C. The reaction was allowed to reach r.t. and stirred overnight. The mixture was filtered and the solution evaporated to dryness under vacuum. The resulting residue was dissolved in DCM and the obtained solution was washed with brine, dried over sodium sulfate, filtered and evaporated to dryness. The crude product was purified by flash-chromatography (eluent:ethyl acetate/cyclohexane 3/7 then 4/6) to give 3.0 g (93% yield) of the title compound as a white solid.