反応式
[ClH:1].[CH3:2][NH2:3].[CH2:4]=O.[C:6](=[O:12])([O:8][CH:9]([CH3:11])[CH3:10])[NH2:7]>C(O)C>[ClH:1].[CH3:2][NH:3][CH2:4][NH:7][C:6](=[O:12])[O:8][CH:9]([CH3:11])[CH3:10]参加物
5
実験手順
To 50 ml of ethanol, 20.3 g (0.3 mole) of methylamine hydrochloride and 30.9 g (0.36 mole) of 37% formaldehyde aqueous solution were added and the mixture was warmed to 35°-40° C. Then, a solution prepared by dissolving 30.9 g (0.3 mole) of isopropyl carbamate in 150 ml of ethanol was added dropwise to the mixture with stirring maintaining the said temperature. After the dropwise addition of the solution, stirring was continued for 1 hour with heating and then the solvent was removed by distillation under reduced pressure. The residue was recrystallized from ethanol to give 42.7 g of isopropyl N-(methylaminomethyl)carbamate hydrochloride having a melting point of 163°-164° C. in yield of 77.8%. ##STR5##
後処理
- temperaturethe mixture was warmed to 35°-40° C
- customThen, a solution prepared
- additionwas added dropwise to the mixture
- temperaturemaintaining the said temperature
- additionAfter the dropwise addition of the solution
- stirringstirring
- temperaturewith heating
- customthe solvent was removed by distillation under reduced pressure
- customThe residue was recrystallized from ethanol
出典と根拠
- ORDレコード
- ord-280fc069745e431a8d0dd3daa014f1cd
- 出典データセット
- uspto-grants-1980_04
- 特許番号
- US04197410
関連ノート
読み込み中…