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tert-Butylhydrazine → HCID 54331272, 화합물

HRID 436763
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HRID 436763 반응식
[C:1]([NH:5][NH2:6])([CH3:4])([CH3:3])[CH3:2].[N:7]([C:16]([N:20]=[C:21]=[O:22])([CH2:18][CH3:19])[CH3:17])=[N:8][C:9]([N:13]=[C:14]=[O:15])([CH2:11][CH3:12])[CH3:10]>CCCCC>[N:7]([C:16]([NH:20][C:21]([NH:6][NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:22])([CH2:18][CH3:19])[CH3:17])=[N:8][C:9]([NH:13][C:14]([NH:6][NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:15])([CH2:11][CH3:12])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 81890tert-ButylhydrazineHCID 53785527HCID 53785527, 화합물

생성물 1

HCID 54331272HCID 54331272, 화합물

시약·촉매·용매 1

HCID 8003Pentane용매

실험 절차

To a stirred solution of 5.8 grams (0.05 moles) of 76% t-butylhydrazine in 30 ml pentane in a 50 ml erlenmeyer flask cooled in a water bath was added 5.6 grams (0.025 moles) of 2,2'-azobis(2-isocyanatobutane) (from Example XXXVI) dropwise over 20 minutes while holding the reaction temperature below 30° C. After the addition was complete, the reaction was stirred for an additional 60 minutes at room temperature and filtered. The filter cake was washed with pentane and dried. The dry white solid weighed 3.3 grams (33% crude yield) and melted at 155°-160° C. with decomposition. The product had a broad strong carbonyl band at 1625- 1675 cm-1 and a broad strong NH band at 3300- 3450 cm-1 in its infrared spectrum and the isocyanate band at 2200 cm-1 was absent.

후처리

  1. customthe reaction temperature below 30° C
  2. additionAfter the addition
  3. filtrationfiltered
  4. washThe filter cake was washed with pentane
  5. customdried

출처 및 근거

ORD 기록
ord-5b89f21457454b679088df3975d59967
출처 데이터셋
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04028344

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