tert-Butyl isocyanate → N-(1-cyano-1-methylethyl)-N'-(1,1-dimethylethyl)urea
反応式
[CH3:1][C:2]([NH2:6])([CH3:5])[C:3]#[N:4].[C:7]([N:11]=[C:12]=[O:13])([CH3:10])([CH3:9])[CH3:8]>>[C:3]([C:2]([NH:6][C:12]([NH:11][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:13])([CH3:5])[CH3:1])#[N:4]参加物
3
実験手順
In a nitrogen atmosphere, 24.8 g. (0.3 mole) 2-methyl-2-aminopropionitrile and 30.7 g. (0.3 mole) t-butyl isocyanate, 97%, are combined and stirred for 5 minutes. At the end of this period, the mixture is filtered and 1 ml. of pyridine is added to the filtrate. This mixture is heated in an oil bath for one and one-half hours, keeping the temperature of the bath below 70°. The solid is recrystallized from methanol:water, 60:40, to give N-(1-cyano-1-methylethyl)-N'-(1,1-dimethylethyl)urea, m.p. 204°-5°; Anal. Calcd. for C9H17N3O; C: 58.99, H: 9.35, N: 22.93; Found: C: 59.21, H: 9.26, N: 22.59.
後処理
- filtrationAt the end of this period, the mixture is filtered
- additionof pyridine is added to the filtrate
- temperatureThis mixture is heated in an oil bath for one and one-half hours
- customthe temperature of the bath below 70°
- customThe solid is recrystallized from methanol
出典と根拠
- ORDレコード
- ord-23879c3033134182b765916ff9ed125b
- 出典データセット
- uspto-grants-1979_05
- 特許番号
- US04156738
反応ノート
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