反应详情

To 1-methoxycarbonylmethyl-1,3-dihydro-isoindole-2-carboxylic acid tert-butyl ester (52.6 g, 180.5 mmol) in MeOH (500 mL) was added 1 N NaOH (199 mL, 199.0 mmol). The mixture is stirred at r.t. for about 48 hours and then concentrated to dryness. The resulting residue was dissolved in water (300 mL) and extracted with diethyl ether (2×). The aqueous portion was acidified to pH 2 with 10% aqueous sodium bisulfate and extracted with EtOAc. The combined organic extracts were dried (MgSO4) and concentrated to dryness to afford about 49.8 g of the final compound (99%). EIS-MS 276 [M−1].

1. concentrationconcentrated to dryness
2. dissolutionThe resulting residue was dissolved in water (300 mL)
3. extractionextracted with diethyl ether (2×)
4. extractionextracted with EtOAc
5. dry with materialThe combined organic extracts were dried (MgSO4)
6. concentrationconcentrated to dryness