反应详情

温度

180 °C

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).

1. temperatureAfter cooling to room temperature
2. filtrationfiltration 1.5 l n-hexane
3. additionwere added
4. filtrationThe resulting precipitate was collected by filtration
5. washAfter washing with hexane
6. dry with materialdrying 34.4 g (77%) N-(2-methoxy-5-morpholin-4-yl-phenyl)-oxalamic acid ethyl ester
7. customwas obtained as greenish crystals, mp.: 95-97° C., MS m/e (%)