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Ammonia → 2-Hydrazino-5,5-Dimethyl-1,3-Diazacyclohex-2-ene Monohydrochloride

HRID 443974
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HRID 443974 반응식
[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]
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참가 물질

3

반응물 2

HCID 222AmmoniaHCID 234662455,5-Dimethyl-1,4,5,6-tetrahydropyrimidin-2-amine hydrochloride

생성물 1

HCID 202453512-Hydrazino-5,5-Dimethyl-1,3-Diazacyclohex-2-ene Monohydrochloride

실험 절차

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.

후처리

  1. customequipped with condenser and magnetic stirring bar
  2. customflushed with argon
  3. additionThere is next added 1.19 parts, 1.5 equivalents
  4. customis obtained
  5. customThe flask is then placed in an oil bath
  6. custompreheated to 115° C
  7. temperatureThe reaction is maintained at 115°-120° C. under a stream of argon for twelve hours
  8. customThe liquid is evaporated at room temperature

출처 및 근거

ORD 기록
ord-7b7db32df3db4c6bbf632ff6a11044f2
출처 데이터셋
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04262122

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