Oxalyl chloride → HCID 15281591、化合物
反応式
[C:1]1(=[O:17])[N:5]([C:6]2[CH:11]=[CH:10][C:9]([CH2:12][C:13](O)=[O:14])=[CH:8][CH:7]=2)[C:4](=[O:16])[CH:3]=[CH:2]1.C(Cl)(=O)C([Cl:21])=O>ClCCl>[C:1]1(=[O:17])[N:5]([C:6]2[CH:11]=[CH:10][C:9]([CH2:12][C:13]([Cl:21])=[O:14])=[CH:8][CH:7]=2)[C:4](=[O:16])[CH:3]=[CH:2]1参加物
4
反応条件
- 温度
- 35 °C
実験手順
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)