Ammonia → 2-Hydrazino-5,5-Dimethyl-1,3-Diazacyclohex-2-ene Monohydrochloride
Reaction equation
[ClH:1].[NH2:2][C:3]1[NH:4][CH2:5][C:6]([CH3:10])([CH3:9])[CH2:7][N:8]=1.[NH3:11]>>[ClH:1].[NH:2]([C:3]1[NH:8][CH2:7][C:6]([CH3:10])([CH3:9])[CH2:5][N:4]=1)[NH2:11]Participants
Procedure
The product (2.60 parts) of Example 1 above, 2-amino-5,5-dimethyl-1,4,5,6-tetrahydropyrimidine hydrochloride, is added to a suitable flask equipped with condenser and magnetic stirring bar, and flushed with argon. There is next added 1.19 parts, 1.5 equivalents, of hydrazine hydrate, and the mixture is stirred until a clear solution is obtained. The flask is then placed in an oil bath preheated to 115° C. Ammonia is evolved almost immediately. The reaction is maintained at 115°-120° C. under a stream of argon for twelve hours. After sitting overnight at room temperature, the flask contains a white, crystalline solid and a small amount of clear, colorless liquid. The liquid is evaporated at room temperature. Resultant yield of 2-hydrazino-5,5-dimethyl-1,4,5,6-tetrahydropyrimidine hydrochloride which is found to be 97% pure is almost quantitative.
Workup
- customequipped with condenser and magnetic stirring bar
- customflushed with argon
- additionThere is next added 1.19 parts, 1.5 equivalents
- customis obtained
- customThe flask is then placed in an oil bath
- custompreheated to 115° C
- temperatureThe reaction is maintained at 115°-120° C. under a stream of argon for twelve hours
- customThe liquid is evaporated at room temperature
Sources & evidence
- ORD record
- ord-7b7db32df3db4c6bbf632ff6a11044f2
- Source dataset
- uspto-grants-1981_04
- Patent number
- US04262122
Reaction notes
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