Methylhydrazine → 4-[1-(t-Butylazo)cyclohexyl]-2-methylsemicarbazide

HRID 436749노트

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HRID 436749 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].[CH3:16][NH:17][NH2:18].[N-]=C=O>CCCCC>[C:1]([N:5]=[N:6][C:7]1([NH:13][C:14](=[O:15])[N:17]([CH3:16])[NH2:18])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 6061MethylhydrazineHCID 105034IsocyanateHCID 214311721-t-Butylazo-1-isocyanatocyclohexane

생성물 1

HCID 214311464-[1-(t-Butylazo)cyclohexyl]-2-methylsemicarbazide

시약·촉매·용매 1

HCID 8003Pentane용매

반응 조건

온도
5 °C

실험 절차

To 8.2 grams (0.0392 moles) of 1-t-butylazo-1-isocyanatocyclohexane stirred with a magnetic stirrer in a 50 ml erlenmeyer flask and cooled to 5° C. was added 1.82 grams (0.0392 moles) of methylhydrazine. The reaction was very rapid and exothermic and became quite viscous. The reaction mixture was diluted with pentane and stirred for an additional 60 minutes at room temperature. The pentane was evaporated under reduced pressure leaving 9.0 grams (90% crude yield) of a yellow solid. The product melted at 169°-171° C. with decomposition. The infrared spectrum of the product contained a strong carbonyl band at 1660 cm-1 and a moderate NH band at 3320 cm-1. The isocyanate band at 2225 cm-1 was absent.

후처리

  1. customThe pentane was evaporated under reduced pressure
  2. customleaving 9.0 grams (90% crude yield) of a yellow solid

출처 및 근거

ORD 기록
ord-8d416c253721430bb3e24f8c083b70fb
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04028344

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