反应详情

温度

23 °C

To a 100 mL round bottom flask containing methyl 1-oxoisoindoline-5-carboxylate (200 mg, 1.046 mmol) was added THF (6 mL) and H2O (2 mL) the mixture was stirred at 23° C. for 2 min. At this time, lithium hydroxide monohydrate (87 μL, 3.14 mmol) was added and the flask was gently heated on aluminum block for 5 min. The solid went into solution and LC/MS showed product formation. The contents of the reaction were poured into HCl (1 M, 15 mL) and extracted with DCM (15 mL). An emulsion formed, the layers separated, and a white solid formed at the boundary of the layers and stuck to the separatory funnel. This material was collected, dissolved in MeOH, and concentrated. After drying under high vacuum for 2 h, the 1-oxoisoindoline-5-carboxylic acid thus obtained was taken on directly to the next reaction without further purification.

1. temperaturethe flask was gently heated on aluminum block for 5 min
2. extractionextracted with DCM (15 mL)
3. customAn emulsion formed
4. customthe layers separated
5. customa white solid formed at the boundary of the layers
6. customThis material was collected
7. dissolutiondissolved in MeOH
8. concentrationconcentrated
9. customAfter drying under high vacuum for 2 h