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Diethyl Ether → 1,3-Dimethyl-2-[2-(1-phenyl-3-indazolyl)vinyl]1H-imidazo[4,5-b]pyrazinium p-toluenesulfonate

HRID 436202
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HRID 436202 반응식
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([O-:10])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[CH3:12][NH+:13]1[C:17]2=[N:18][CH:19]=[CH:20][N:21]=[C:16]2[N:15]([CH3:22])[CH:14]1[CH3:23].[CH:24]([C:26]1[C:34]2[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=2)[N:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[N:27]=1)=O.CCOCC>C(OC(=O)C)(=O)C>[C:1]1([CH3:11])[CH:2]=[CH:3][C:4]([S:7]([O-:10])(=[O:8])=[O:9])=[CH:5][CH:6]=1.[CH3:22][NH+:15]1[C:16]2=[N:21][CH:20]=[CH:19][N:18]=[C:17]2[N:13]([CH3:12])[CH:14]1[CH:23]=[CH:24][C:26]1[C:34]2[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=2)[N:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[N:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 214547813-Formyl-1-phenylindazoleHCID 214547841,2,3-trimethyl-1H-imidazo[4,5-b]-pyrazinium p-toluenesulfonate

생성물 1

HCID 737919641,3-Dimethyl-2-[2-(1-phenyl-3-indazolyl)vinyl]1H-imidazo[4,5-b]pyrazinium p-toluenesulfonate

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

A mixture of 1,2,3-trimethyl-1H-imidazo[4,5-b]-pyrazinium p-toluenesulfonate (1.67 g, 0.050 mole) and 3-formyl-1-phenylindazole (1.11 g, 0.050 mole) is heated together in acetic anhydride (15 ml) at reflux for 30 minutes. After chilling, ether (500 ml) is added and the solid which separates is filtered off and dried. Yield 1.92 g, (72%). After recrystallization from water the yield of dye is 0.55 g (41%).

후처리

  1. temperatureat reflux for 30 minutes
  2. temperatureAfter chilling
  3. filtrationthe solid which separates is filtered off
  4. customdried
  5. customAfter recrystallization from water the yield of dye

출처 및 근거

ORD 기록
ord-6530c8186d724382beb1e04e3647c743
출처 데이터셋
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04007170

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