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4-Fluorobenzoic Acid → HCID 68750889、化合物

HRID 1864780
ノート
印刷プレビュー

反応式

HRID 1864780 の反応式
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:25][Si:26]([CH3:76])([CH3:75])[CH2:27][CH2:28][O:29][C:30]([N:32]1[CH2:37][CH2:36][CH:35]([NH:38][CH2:39][C:40]2[CH:45]=[C:44]([C:46]3[CH:73]=[CH:72][C:49]4[N:50]([C:53]([C:66]5[CH:71]=[CH:70][CH:69]=[CH:68][CH:67]=5)([C:60]5[CH:65]=[CH:64][CH:63]=[CH:62][CH:61]=5)[C:54]5[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=5)[N:51]=[N:52][C:48]=4[CH:47]=3)[CH:43]=[CH:42][C:41]=2[F:74])[CH2:34][CH2:33]1)=[O:31].[F:77][C:78]1[CH:86]=[CH:85][C:81]([C:82](O)=[O:83])=[CH:80][CH:79]=1.C(N(C(C)C)CC)(C)C>C(OCC)(=O)C>[CH3:25][Si:26]([CH3:76])([CH3:75])[CH2:27][CH2:28][O:29][C:30]([N:32]1[CH2:33][CH2:34][CH:35]([N:38]([C:82](=[O:83])[C:81]2[CH:85]=[CH:86][C:78]([F:77])=[CH:79][CH:80]=2)[CH2:39][C:40]2[CH:45]=[C:44]([C:46]3[CH:73]=[CH:72][C:49]4[N:50]([C:53]([C:54]5[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=5)([C:60]5[CH:61]=[CH:62][CH:63]=[CH:64][CH:65]=5)[C:66]5[CH:67]=[CH:68][CH:69]=[CH:70][CH:71]=5)[N:51]=[N:52][C:48]=4[CH:47]=3)[CH:43]=[CH:42][C:41]=2[F:74])[CH2:36][CH2:37]1)=[O:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 99734-Fluorobenzoic AcidHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 68796575HCID 68796575、化合物

生成物 1

HCID 68750889HCID 68750889、化合物

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

実験手順

HATU was added to a solution of 4-[2-fluoro-5-(1-trityl-1H-benzotriazol-5-yl)-benzylamino]-piperidine-1-carboxylic acid 2-trimethylsilany-1-ethyl ester, 4-fluorobenzoic acid and diisopropylethylamine and the resulting mixture stirred at ambient temperature overnight. The mixture was diluted with ethyl acetate washed with 1 M sodium carbonate solution. The layers were separated and the aqueous phase extracted with ethyl acetate. The combined organic phases were washed with brine, dried over magnesium sulfate, filtered and concentrated to leave the crude product. Chromatography (elution with diethyl ether/hexane, followed by ethyl acetate/hexane) provided 740 mg of product.

後処理

  1. washwashed with 1 M sodium carbonate solution
  2. customThe layers were separated
  3. extractionthe aqueous phase extracted with ethyl acetate
  4. washThe combined organic phases were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto leave the crude product
  9. washChromatography (elution with diethyl ether/hexane, followed by ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-481533e7164544fc9cba62420738ac5e
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07625889B2

反応ノート

読み込み中…

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