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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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4,7-dimethyl-2,3-dihydro-1H-indole-2,3-dione → 3-(4-Fluoro-benzyl)-5,8-dimethyl-9H-1,2,3a,4,9,10-hexaaza-cyclopenta[b]fluorene

HRID 1822906
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인쇄 미리보기

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HRID 1822906 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([CH3:11])=[C:7]2[C:3]=1[C:4](=O)[C:5](=O)[NH:6]2.[F:14][C:15]1[CH:28]=[CH:27][C:18]([CH2:19][C:20]2[N:21]([NH2:26])[C:22]([NH2:25])=[N:23][N:24]=2)=[CH:17][CH:16]=1>C(O)CO.O>[F:14][C:15]1[CH:28]=[CH:27][C:18]([CH2:19][C:20]2[N:21]3[C:22]([N:25]=[C:5]4[C:4](=[N:26]3)[C:3]3[C:7](=[C:8]([CH3:11])[CH:9]=[CH:10][C:2]=3[CH3:1])[NH:6]4)=[N:23][N:24]=2)=[CH:17][CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 32649314,7-dimethyl-2,3-dihydro-1H-indole-2,3-dioneHCID 219193225-[(4-Fluorophenyl)methyl]-4H-1,2,4-triazole-3,4-diamine

생성물 1

HCID 1355074463-(4-Fluoro-benzyl)-5,8-dimethyl-9H-1,2,3a,4,9,10-hexaaza-cyclopenta[b]fluorene

시약·촉매·용매 2

HCID 174Ethylene Glycol용매HCID 962Water용매

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온도
125 °C

실험 절차

According to the general cyclization procedure (for Example 27), 0.60 mmol of 4,7-dimethyl-1H-indole-2,3-dione (105 mg) and 0.70 mmol of (4-fluoro-benzyl)-[1,2,4]triazole-3,4-diamine (145 mg) in 2 mL of ethylene glycol was stirred at 125° C. overnight (18 hr). The mixture was cooled to room temperature, diluted with water (10 mL), stirred for 15 min. The precipitated product was collected by filtration, washed with MeOH+water 1:1. Dried on high vacuum. The crude product (187 mg) was suspended in anhydrous ethanol (6 mL), heated to reflux, sonicated while hot, allowed to cool overnight, filtered, washed with ice-cold methanol, filtered and dried on high vacuum.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. stirringstirred for 15 min
  3. filtrationThe precipitated product was collected by filtration
  4. washwashed with MeOH+water 1:1
  5. customDried on high vacuum
  6. temperatureheated
  7. temperatureto reflux
  8. customsonicated while hot,
  9. temperatureto cool overnight
  10. filtrationfiltered
  11. washwashed with ice-cold methanol
  12. filtrationfiltered
  13. customdried on high vacuum

출처 및 근거

ORD 기록
ord-79e6422ddd6943a281b9842203536ba5
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07037909B2

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