反应详情

温度

35 °C

1.0 g (4.33 mmol) of p-maleinimidophenylacetic acid were suspended in 25 ml of dichloromethane and diluted with a 2.5-fold excess of oxalic acid dichloride (1.37 g, 945 μl; 10.82 mmol). The reaction mixture was heated to 30-40° C. with the exclusion of moisture and stirred for 15 h. Then the solvent was removed under a vacuum and dried under a high vacuum. Crystallization from toluene yielded a yellow powder (yield: 59%); melting point: 154° C.; Rf-value: 0.29 (acetic ester/hexane 4/1); Elementary analysis: calculated: C: 58.91% H: 3.30% N: 5.75%, Cl: 14.49%; (C12H8NO3Cl) found: C: 60.61% H: 3.64% N: 5.13% Cl: 13.80%.

1. customThen the solvent was removed under a vacuum
2. customdried under a high vacuum
3. customCrystallization from toluene