Diethyl Oxalate → HCID 21137088、化合物
反応式
[C:1]([O:8][CH2:9][CH3:10])(=[O:7])[C:2]([O:4]CC)=O.[CH3:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)=[CH:15][C:14]=1[NH2:25]>>[CH2:9]([O:8][C:1](=[O:7])[C:2]([NH:25][C:14]1[CH:15]=[C:16]([N:19]2[CH2:20][CH2:21][O:22][CH2:23][CH2:24]2)[CH:17]=[CH:18][C:13]=1[O:12][CH3:11])=[O:4])[CH3:10]参加物
3
反応条件
- 温度
- 180 °C
実験手順
139 ml (1015 mmol) Diethyl oxalate were heated to 120° C. 30.3 g (145 mmol) 2-methoxy-5-morpholin-4-yl-phenylamine were added very cautiously in small quantities and the mixture was heated for 90 minutes at 180° C. After cooling to room temperature and filtration 1.5 l n-hexane were added. The resulting precipitate was collected by filtration. After washing with hexane and drying 34.4 g (77%) N-(2-methoxy-5-morpholin-4-yl-phenyl)-oxalamic acid ethyl ester was obtained as greenish crystals, mp.: 95-97° C., MS m/e (%): 309 (M+H+, 100).
後処理
- temperatureAfter cooling to room temperature
- filtrationfiltration 1.5 l n-hexane