Dimethylformamide → HCID 89619455、化合物
反応式
[Cl:1][C:2]1[CH:3]=[C:4](C(C(O)=O)C(O)=O)[CH:5]=[C:6]([Cl:8])[CH:7]=1.Cl[CH2:17][Cl:18].[C:19](Cl)(=O)[C:20]([Cl:22])=[O:21].CN(C)C=[O:28]>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:19]([C:17]([Cl:18])=[O:28])[C:20]([Cl:22])=[O:21])[CH:5]=[C:6]([Cl:8])[CH:7]=1参加物
5
実験手順
A 4-necked 500-mL flask equipped with overhead stirrer, condenser, thermometer, and addition funnel was charged with 2-(3,5-dichlorophenyl)propanedioic acid (21.8 g, 87.6 mmol), anhydrous dichloromethane (300 mL), and N,N-dimethylformamide (0.1 mL). To this stirred solution was added oxalyl chloride (19 mL, 217 mmol) over 10 min at room temperature. The mixture was stirred at room temperature for 1 hr, then refluxed for 2.5 h under nitrogen. The resulting yellow solution was concentrated under reduced pressure (20 mmHg) at a temperature of 25° C. to yield the crude product as an orange oil. The resulting material was used directly in the next step.