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Triethylamine → HCID 18982007, 화합물

HRID 1440783
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HRID 1440783 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 32484DiisopropylanilineHCID 199401P,P-Diphenylphosphinic azideHCID 18982012HCID 18982012, 화합물

생성물 1

HCID 18982007HCID 18982007, 화합물수율 90.9%

시약·촉매·용매 2

HCID 962Water용매
HCID 10008
Fluorobenzene
용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-f5eca9916cc24f6f9007c595ed1b563b
출처 데이터셋
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05500424

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