Diethyl Oxalate → HCID 21137088, 화합물
반응식
[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]참가 물질
3
반응 조건
- 온도
- 180 °C
실험 절차
139 ml (1015 mmol) Diethyl oxalate was heated to 120° C. 30.3 g (145 mmol) 2-methoxy-5-morpholin-4-yl-phenylamine was 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 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, M.p.: 95–97° C., MS m/e (%): 309 (M+H+, 100).
후처리
- temperatureAfter cooling to room temperature