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Triethylamine → HCID 18982007、化合物

HRID 1440783
ノート
印刷プレビュー

反応式

HRID 1440783 の反応式
[C:1]1([C:7]2[C:12](C(O)=O)=[CH:11][CH:10]=[C:9]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:29])C=CC=CC=1.C([N:41]([CH2:44]C)CC)C.[CH:46]([C:49]1[CH:55]=[CH:54][CH:53]=[C:52]([CH:56]([CH3:58])[CH3:57])[C:50]=1[NH2:51])([CH3:48])[CH3:47]>FC1C=CC=CC=1.O>[CH:56]([C:52]1[CH:53]=[CH:54][CH:55]=[C:49]([CH:46]([CH3:48])[CH3:47])[C:50]=1[NH:51][C:44]([NH:41][C:12]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8][C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:10][CH:11]=1)=[O:29])([CH3:58])[CH3:57]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 32484DiisopropylanilineHCID 199401P,P-Diphenylphosphinic azideHCID 18982012HCID 18982012、化合物

生成物 1

HCID 18982007HCID 18982007、化合物収率 90.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 10008
Fluorobenzene
溶媒

実験手順

To a stirred mixture of 551 mg of 2,6-diphenyl-3-pyridinecarboxylic acid and 0.52 cc of diphenylphosphoryl azide in 6 cc of fluorobenzene was added dropwise 0.29 cc of triethylamine at room temperature. The resulting mixture was stirred at room temperature for 30 minutes and then heated at a temperature of 65°-70° C. for 10 minutes. After cooling, 0.45 cc of 2,6-diisopropylaniline was added and the resulting mixture was heated at a temperature of 70° C. for 1.5 hours. After cooling, water was added to the reaction mixture and extracted with chloroform. The extract was dried over magnesium sulfate, and distilled to remove the solvent. The crude product thus obtained was purified by a silica gel column chromatography (eluent: chloroform) to obtain 817 mg of compound 61.

後処理

  1. temperatureheated at a temperature of 65°-70° C. for 10 minutes
  2. temperatureAfter cooling
  3. temperaturethe resulting mixture was heated at a temperature of 70° C. for 1.5 hours
  4. temperatureAfter cooling
  5. extractionextracted with chloroform
  6. dry with materialThe extract was dried over magnesium sulfate
  7. distillationdistilled
  8. customto remove the solvent
  9. customThe crude product thus obtained
  10. customwas purified by a silica gel column chromatography (eluent: chloroform)

出典と根拠

ORDレコード
ord-f5eca9916cc24f6f9007c595ed1b563b
出典データセット
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05500424

反応ノート

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