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Hydrazine → 1,2-Di[1-(t-butylazo)cyclohexylaminocarbonyl]hydrazine

HRID 436751
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HRID 436751 반응식
[C:1]([N:5]=[N:6][C:7]1([N:13]=[C:14]=[O:15])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([CH3:4])([CH3:3])[CH3:2].[NH2:16][NH2:17]>CCCCC>[C:1]([N:5]=[N:6][C:7]1([NH:13][C:14]([NH:16][NH:17][C:14]([NH:13][C:7]2([N:6]=[N:5][C:1]([CH3:4])([CH3:3])[CH3:2])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)=[O:15])=[O:15])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 214311721-t-Butylazo-1-isocyanatocyclohexane

생성물 1

HCID 214312961,2-Di[1-(t-butylazo)cyclohexylaminocarbonyl]hydrazine

시약·촉매·용매 1

HCID 8003Pentane용매

실험 절차

To 9.27 grams (0.044 moles) of 1-t-butylazo-1-isocyanatocyclohexane stirred with a magnetic stirrer in a 50 ml erlenmeyer flask was added 0.74 grams (0.022 moles) of 97% hydrazine. The reaction mixture rapidly became a solid and pentane was added to slurry the mixture. The slurry was then stirred for 60 minutes at room temperature and filtered. The filter cake was dried leaving 9.5 grams (95% crude yield) of a white powder. The product melted at 195°-197° C. with decomposition. The infrared spectrum of the product contained a strong carbonyl band at 1665 cm-1 and a broad NH band at 3350 cm-1 and a weaker band at 3080 cm-1.

후처리

  1. additionwas added to slurry the mixture
  2. filtrationfiltered
  3. customThe filter cake was dried
  4. customleaving 9.5 grams (95% crude yield) of a white powder

출처 및 근거

ORD 기록
ord-b3b237586c7941aba7cc4abe90eeedc1
출처 데이터셋
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04028344

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