Dimethylamine → 1,1-Dimethyl-2-(2-morpholinophenyl)guanidine
反応式
I.CS[C:4](=[NH:18])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[N:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1.[CH3:19][NH:20][CH3:21]>C(O)C>[CH3:19][N:20]([CH3:21])[C:4]([NH2:18])=[N:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[N:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1参加物
4
実験手順
A mixture of 2-methyl-1-(2-morpholinophenyl)-2-thiopseudourea hydroiodide (1 g), dimethylamine (1 ml of a 33% solution in ethanol) and ethanol (2 ml) was kept at ambient temperature for 48 days. The mixture was then cooled in an ice bath. The resulting solid was separated by filtration, treated with dilute aqueous sodium hydroxide solution (5 ml) and the resulting mixture extracted with dichloromethane (2×50 ml). The extract was washed with brine, dried and the solvent removed by evaporation to give 1,1-dimethyl-2-(2-morpholinophenyl)guanidine (m.p. 143°-144° C.) which was recrystallised from hexane.
後処理
- temperatureThe mixture was then cooled in an ice bath
- customThe resulting solid was separated by filtration
- additiontreated with dilute aqueous sodium hydroxide solution (5 ml)
- extractionthe resulting mixture extracted with dichloromethane (2×50 ml)
- washThe extract was washed with brine
- customdried
- customthe solvent removed by evaporation
出典と根拠
- ORDレコード
- ord-67e7f2b7501747a6851c57bdc98c64bd
- 出典データセット
- uspto-grants-1994_12
- 特許番号
- US05373008
反応ノート
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