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4-Amino-m-cresol → Ethyl 3-methoxy-7-(4-hydroxy-2-methylphenylamino)thieno-[3,2-b]pyridine-6-carboxylate hydrochloride

HRID 2107625
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HRID 2107625 반응식
[CH3:1][O:2][C:3]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:11]([Cl:12])=[C:6]2[S:5][CH:4]=1.[OH:18][C:19]1[CH:25]=[CH:24][C:22]([NH2:23])=[C:21]([CH3:26])[CH:20]=1>C1(OC)C=CC=CC=1>[ClH:12].[CH3:1][O:2][C:3]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:11]([NH:23][C:22]3[CH:24]=[CH:25][C:19]([OH:18])=[CH:20][C:21]=3[CH3:26])=[C:6]2[S:5][CH:4]=1
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참가 물질

4

반응물 2

HCID 178194-Amino-m-cresolHCID 23046152Ethyl 3-methoxy-7-chlorothieno[3,2-b]pyridine-6-carboxylate

생성물 1

HCID 23046154Ethyl 3-methoxy-7-(4-hydroxy-2-methylphenylamino)thieno-[3,2-b]pyridine-6-carboxylate hydrochloride

시약·촉매·용매 1

HCID 7519Anisole용매

실험 절차

Ethyl 3-methoxy-7-chlorothieno[3,2-b]pyridine-6-carboxylate (1.5 g, 0.0055 mol) and 4-hydroxy-2-methylaniline (1.36 g, 0.011 mol) in anisole (30 ml) were heated under reflux in an inert atmosphere for thirty hours. The solid obtained on cooling was collected by filtration and recrystallised from ethanol to give a brown crystalline solid, 1.09 g. Recrystallisation from ethanol after filtration through charcoal gave the title compound, 0.63 g, m.p. 286°-288°.

후처리

  1. temperatureunder reflux in an inert atmosphere for thirty hours
  2. customThe solid obtained
  3. temperatureon cooling
  4. filtrationwas collected by filtration
  5. customrecrystallised from ethanol
  6. customto give a brown crystalline solid, 1.09 g
  7. customRecrystallisation from ethanol
  8. filtrationafter filtration through charcoal

출처 및 근거

ORD 기록
ord-f8d7e40227da4da3ade15a2ccaae83af
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04935431

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