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Methanol → 5-(4-Methoxyphenyl)-2-(1,2,3,4-tetrahydroquinolin-7-yl)thiazole-4-carboxylic acid

HRID 2178214
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HRID 2178214 반응식
C([N:4]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([C:14]3[S:15][C:16]([C:24]4[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[CH:26][CH:25]=4)=[C:17]([C:19]([O:21]CC)=[O:20])[N:18]=3)[CH:12]=2)[CH2:7][CH2:6][CH2:5]1)(=O)C.[OH-].[K+].CO>O>[CH3:31][O:30][C:27]1[CH:28]=[CH:29][C:24]([C:16]2[S:15][C:14]([C:11]3[CH:12]=[C:13]4[C:8]([CH2:7][CH2:6][CH2:5][NH:4]4)=[CH:9][CH:10]=3)=[N:18][C:17]=2[C:19]([OH:21])=[O:20])=[CH:25][CH:26]=1
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참가 물질

5

반응물 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 59418743Ethyl 2-(1-acetyl-1,2,3,4-tetrahydroquinolin-7-yl)-5-(4-methoxyphenyl)thiazole-4-carboxylate

생성물 1

HCID 594187575-(4-Methoxyphenyl)-2-(1,2,3,4-tetrahydroquinolin-7-yl)thiazole-4-carboxylic acid수율 86%

시약·촉매·용매 1

HCID 962Water용매

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온도
55 °C

실험 절차

To ethyl 2-(1-acetyl-1,2,3,4-tetrahydroquinolin-7-yl)-5-(4-methoxyphenyl)thiazole-4-carboxylate (1K) (0.483 g, 1.11 mmol) and KOH (1.24 g, 22.1 mmol) was added MeOH (10 mL) and water (45 mL). The reaction mixture was allowed to heat to 55° C. and stirred 48 hours. The reaction was monitored by LCMS. To the reaction mixture was added (0.5 g, 8.9 mmol). The reaction mixture was allowed to heat to 55° C. and stirred for 24 hours. The reaction mixture was cooled to rt and concentrated under reduced pressure. To the crude residue was added EtOAc and water. The layers were separated and the aqueous extract was acidified to ˜pH6 with 1N HCl and extracted with EtOAc. The combined organic extracts were washed sequentially with water, brine, dried over MgSO4, filtered, and concentrated under reduced pressure to provide 0.350 g (86%) of the desired product 5-(4-methoxyphenyl)-2-(1,2,3,4-tetrahydroquinolin-7-yl)thiazole-4-carboxylic acid (1L): LC/MS (APCI): m/z 367.0 (M+H).

후처리

  1. additionTo the reaction mixture was added (0.5 g, 8.9 mmol)
  2. temperatureto heat to 55° C.
  3. stirringstirred for 24 hours
  4. temperatureThe reaction mixture was cooled to rt
  5. concentrationconcentrated under reduced pressure
  6. additionTo the crude residue was added EtOAc and water
  7. customThe layers were separated
  8. extractionthe aqueous extract
  9. extractionextracted with EtOAc
  10. washThe combined organic extracts were washed sequentially with water, brine
  11. dry with materialdried over MgSO4
  12. filtrationfiltered
  13. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-39550be039684684ac5bd943ee954a3c
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09067928B2

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