Diethyl Ether → HCID 6618973、化合物

温度

0 °C

According to the procedure of B. Agai, et al., Tetrahedron, 32, 839, (1976), to a cooled (0° C.), stirred suspension of 2-(2-aminoanilino)ethanol (30.4 g, 0.200 mol) in MeOH (100 mL) was added a solution of CH3NCS (14.6 g, 0.200 mol) in MeOH (60 mL) dropwise. The resulting mixture was stirred at room temperature for 4 hours and then heated under reflux for 15 minutes. CH3I (28.4 g, 0.200 mol) was added and the mixture was heated under reflux for 10 minutes, cooled to room temperature and stirred for 2 hours. Ether (200 mL) was added and the resulting precipitate was collected by filtration, taken up in nBuOH (140 mL), and heated under reflux for 10 hours. The mixture was cooled in the freezer for 3 hours and the white crystals were filtered. The material was dissolved in H2O and the solution was neutralized with 10% aqueous K 2 CO3. The white solid was collected by filtration to give 8.2 g (21%) of product m.p. >200° C.

1. stirringThe resulting mixture was stirred at room temperature for 4 hours
2. temperatureheated
3. temperatureunder reflux for 15 minutes
4. temperaturethe mixture was heated
5. temperatureunder reflux for 10 minutes
6. temperaturecooled to room temperature
7. stirringstirred for 2 hours
8. filtrationthe resulting precipitate was collected by filtration
9. temperatureheated
10. temperatureunder reflux for 10 hours
11. temperatureThe mixture was cooled in the freezer for 3 hours
12. filtrationthe white crystals were filtered
13. dissolutionThe material was dissolved in H2O
14. filtrationThe white solid was collected by filtration

ORDレコード

ord-aa191f88c31d41e39f267e3acfdfff25

出典データセット

uspto-grants-1992_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05149700