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Triethylamine → 1,1'-Biphenyl-4-yl-(4H, 10H-3a,5,9-triaza-benzo[f]azulen-9-yl)-methanone

HRID 1354030
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HRID 1354030 반응식
[CH:1]1[CH:2]=[CH:3][N:4]2[C:10]=1[CH2:9][NH:8][C:7]1[CH:11]=[CH:12][CH:13]=[N:14][C:6]=1[CH2:5]2.[C:15]1([C:21]2[CH:29]=[CH:28][C:24]([C:25](Cl)=[O:26])=[CH:23][CH:22]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[C:21]1([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:22]=[CH:23][C:24]([C:25]([N:8]2[CH2:9][C:10]3[N:4]([CH:3]=[CH:2][CH:1]=3)[CH2:5][C:6]3[N:14]=[CH:13][CH:12]=[CH:11][C:7]2=3)=[O:26])=[CH:28][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 841514-Phenylbenzoyl chlorideHCID 167520349,10-dihydro-4H-3a, 5,9-triaza-benzo[f]azulene

생성물 1

HCID 101557261,1'-Biphenyl-4-yl-(4H, 10H-3a,5,9-triaza-benzo[f]azulen-9-yl)-methanone

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A stirred mixture of 9,10-dihydro-4H-3a,5,9-triaza-benzo[f]azulene of Step D (0.54 mmol), 4-phenylbenzoylchloride (1.08 mmol) and triethylamine (1.08 mmol) in toluene was refluxed under nitrogen for 72 hours. The reaction was cooled and the solvent removed in vacuo. Chromatography of the residue over silica gel Merck-60 with a solvent gradient from 5 to 20% ethyl acetate in hexane provided the title compound as a tan solid.

후처리

  1. temperaturewas refluxed under nitrogen for 72 hours
  2. temperatureThe reaction was cooled
  3. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-8b5878cac84d467bba9b6239dd3e2935
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07223752B2

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