反应详情

To a solution of 5-[3-tert-butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyryl]-5,6-dihydro-4H-2,5,10b-triaza-benzo[e]azulene-3-carboxylic acid ethyl ester (100 mg, 0.17 mmol) in THF (5 mL) and water (5 mL), was added lithium hydroxide (43 mg, 1.03 mmol). The reaction mixture was stirred at r.t. overnight. After the completion of the reaction as confirmed by TLC, the reaction mixture was cooled to 0° C. and neutralized with 10% HCl solution to pH˜4. The compound was extracted with ethylacetate (15 mL). The organic layer was washed with water, separated, dried over Na2SO4 and concentrated in vacuo to afford 5-[3-tert-butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyryl]-5,6-dihydro-4H-2,5,10b-triaza-benzo[e]azulene-3-carboxylic acid (85 mg, 89%) as a viscous gel which was used without further purification for the next step.

1. customAfter the completion of the reaction
2. extractionThe compound was extracted with ethylacetate (15 mL)
3. washThe organic layer was washed with water
4. customseparated
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo