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Trimesoyl chloride → 1,3,5-Tris-(5-[1,10]phenanthroline-2-yl-[1,3,4]oxadiazol-2-yl)-benzene

HRID 1180687
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HRID 1180687 반응식
N1[C:5]([C:6]2[CH:19]=[CH:18][C:17]3[C:8](=[C:9]4[C:14](=[CH:15][CH:16]=3)[CH:13]=[CH:12][CH:11]=[N:10]4)[N:7]=2)=[N:4][N:3]=N1.[C:20]1([C:32](Cl)=[O:33])[CH:25]=[C:24]([C:26](Cl)=[O:27])[CH:23]=[C:22]([C:29](Cl)=[O:30])[CH:21]=1>N1C=CC=CC=1>[N:7]1[C:8]2[C:17](=[CH:16][CH:15]=[C:14]3[C:9]=2[N:10]=[CH:11][CH:12]=[CH:13]3)[CH:18]=[CH:19][C:6]=1[C:5]1[O:33][C:32]([C:20]2[CH:25]=[C:24]([C:26]3[O:27][C:5]([C:6]4[CH:19]=[CH:18][C:17]5[C:8](=[C:9]6[C:14](=[CH:15][CH:16]=5)[CH:13]=[CH:12][CH:11]=[N:10]6)[N:7]=4)=[N:4][N:3]=3)[CH:23]=[C:22]([C:29]3[O:30][C:5]([C:6]4[CH:19]=[CH:18][C:17]5[C:8](=[C:9]6[C:14](=[CH:15][CH:16]=5)[CH:13]=[CH:12][CH:11]=[N:10]6)[N:7]=4)=[N:4][N:3]=3)[CH:21]=2)=[N:3][N:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 78138Trimesoyl chlorideHCID 178420729HCID 178420729, 화합물

생성물 1

HCID 589799681,3,5-Tris-(5-[1,10]phenanthroline-2-yl-[1,3,4]oxadiazol-2-yl)-benzene수율 44.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
85 °C

실험 절차

To a flask was added a mixture of 15 g 2-(1H-tetrazol-5-yl)-[1,10]phenanthroline and 300 ml pyridine. The mixture was then heated to 80-90° C., and 4.86 g 1,3,5 benzene tricarbonyl chloride was added. Subsequently, the mixture solution was heated to 110° C. and stirred overnight. After completion of reaction, as shown in scheme 8, the reaction mixture was filtered to collect solids. The solids was washed by pyridine and CH2Cl2 respectively, and then dried on oven to obtain products 6.6 g (yield=44.1%). MS(m/z, FAB+), 888, 810, 521, 444, 155.

후처리

  1. additionTo a flask was added
  2. temperatureSubsequently, the mixture solution was heated to 110° C.
  3. customAfter completion of reaction
  4. filtrationthe reaction mixture was filtered
  5. customto collect solids
  6. washThe solids was washed by pyridine and CH2Cl2 respectively
  7. customdried on oven

출처 및 근거

ORD 기록
ord-42c58dc405e44091894b97aeb08b019a
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07282586B1

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