Aniline → HCID 20064831, 화합물

HRID 652694노트

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HRID 652694 반응식
[S:1](=[O:5])(=[O:4])([OH:3])[O-:2].[C:6]1([C:12]2[CH:17]=[C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:15]=[C:14]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[O+]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[CH2:30]([C:44]1[CH:50]=[CH:49][C:47]([NH2:48])=[CH:46][CH:45]=1)[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43].NC1C=CC=CC=1>C(O)C>[S:1](=[O:3])(=[O:2])([OH:5])[O-:4].[CH2:30]([C:44]1[CH:45]=[CH:46][C:47]([N+:48]2[C:12]([C:6]3[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=3)=[CH:17][C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:15][C:14]=2[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[CH:49][CH:50]=1)[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43]

참가 물질

5

반응물 3

HCID 6115AnilineHCID 145224p-TetradecylanilineHCID 117291982,4,6-Triphenylpyrylium Hydrogensulfate

생성물 1

HCID 20064831HCID 20064831, 화합물수율 21%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
90 °C

실험 절차

In a 500-ml round-bottom flask is placed 2.03 g (0.005 mole) of 2,4,6-triphenylpyrylium bisulfate. To this is added 150 ml of ethanol followed by 2.90 g (0.01 mole) of p-tetradecylaniline. This mixture is heated at 90° C. for about 8 hours and then allowed to cool. Upon cooling some of the starting aniline separates and is removed by filtration. The ethanol is then removed to give a yellow waxy substance which is rinsed with ether to remove any excess pyrylium. The resulting product is then dissolved in acetonitrile to remove any aniline still present. The acetonitrile is then stripped and the product is rinsed a final time with ether. The final product is a yellow crystal which turns a pale yellow color upon grinding. The yield is 0.71 g (0.00105 mole) of N-(p-tetradecylphenyl)-2,4,6-triphenylpyridinium bisulfate (yield 21 percent).

후처리

  1. customIn a 500-ml round-bottom flask is placed
  2. temperatureto cool
  3. customis removed by filtration
  4. customThe ethanol is then removed
  5. customto give a yellow waxy substance which
  6. washis rinsed with ether
  7. customto remove any excess pyrylium
  8. dissolutionThe resulting product is then dissolved in acetonitrile
  9. customto remove any aniline still present
  10. washthe product is rinsed a final time with ether
  11. customupon grinding

출처 및 근거

ORD 기록
ord-7d144bcd57b248939dc8e3dc682ad031
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04672118

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