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Aniline → HCID 53862970, 화합물

HRID 436765
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HRID 436765 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:8]([C:17]([N:21]=[C:22]=[O:23])([CH2:19][CH3:20])[CH3:18])=[N:9][C:10]([N:14]=[C:15]=[O:16])([CH2:12][CH3:13])[CH3:11]>CCCCC>[N:8]([C:17]([NH:21][C:22]([NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:23])([CH2:19][CH3:20])[CH3:18])=[N:9][C:10]([NH:14][C:15]([NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:16])([CH2:12][CH3:13])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6115AnilineHCID 53785527HCID 53785527, 화합물

생성물 1

HCID 53862970HCID 53862970, 화합물

시약·촉매·용매 1

HCID 8003Pentane용매

실험 절차

To a stirred solution of 4.44 grams (0.0476 moles) of aniline in 30 ml of pentane in a 50 ml erlenmeyer flask cooled in a water bath was added 5.33 grams (0.0236 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 1.5 grams (15% crude yield) and melted at 118°-120° C. The product had a strong carbonyl band at 1680 cm-1 and NH peaks at 3220 and 3420 cm-1 in its infrared spectrum and there was no isocyanate band at 2200 cm-1.

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-821fc30c4c8f45cdb028edcf30854cda
출처 데이터셋
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04028344

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