tert-Butyl isocyanate → N-(1-cyano-1-methylethyl)-N'-(1,1-dimethylethyl)urea

반응식

[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]

참가 물질

반응물 2

HCID 62412tert-Butyl isocyanate

HCID 880222-Amino-2-methylpropionitrile

생성물 1

HCID 21316843N-(1-cyano-1-methylethyl)-N'-(1,1-dimethylethyl)urea

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록: ord-23879c3033134182b765916ff9ed125b
출처 데이터셋: uspto-grants-1979_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04156738

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