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Phenylhydrazine → 4-[1-(t-Butylazo)cyclohexyl]-1-phenylsemicarbazide

HRID 436746
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반응식

HRID 436746 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].[C:16]1([NH:22][NH2:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CCCCC>[C:1]([N:5]=[N:6][C:7]1([NH:13][C:14](=[O:15])[NH:23][NH:22][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[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 7516PhenylhydrazineHCID 214311721-t-Butylazo-1-isocyanatocyclohexane

생성물 1

HCID 214311824-[1-(t-Butylazo)cyclohexyl]-1-phenylsemicarbazide

시약·촉매·용매 1

HCID 8003Pentane용매

실험 절차

To 6.6 grams (0.0315 moles) of 1-t-butylazo-1-isocyanatocyclohexane cooled to 5° C. and stirred with a magnetic stirrer in a 50 ml erlenmeyer flask was added dropwise 3.42 grams (0.0315 moles) of phenylhydrazine. The reaction was very exothermic and rapid. Pentane was added to slurry the solid product and the slurry was filtered. The white solid filter cake was air dried and weighed 10.0 grams (100% crude yield). The product melted at 140°-142° C. with decomposition. The infrared spectrum of the product contained a strong carbonyl band at 1670 cm-1 and NH bands at 3100, 3230 and 3320 cm-1. The isocyanate band at 2225 cm-1 was absent.

후처리

  1. filtrationthe slurry was filtered
  2. filtrationThe white solid filter cake
  3. customdried

출처 및 근거

ORD 기록
ord-20e49b29087a41aa99a4bb869c9ff367
출처 데이터셋
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04028344

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