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Ethanolamine → 2-(2-o-Tolyl-chroman-6-yloxy)-thiazole-5-carboxylic acid (2-hydroxy-ethyl)-amide

HRID 1404207
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1404207
[Li+].[C:2]1([CH3:27])[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[CH2:17][CH2:16][C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:18][C:19]3[S:20][C:21]([C:24]([O-])=[O:25])=[CH:22][N:23]=3)[CH:14]=2)[O:9]1.CN(C)C=O.ON1C2C=CC=CC=2N=N1.C[N:44]1CC[O:47][CH2:46][CH2:45]1.C(CN)O>O>[OH:47][CH2:46][CH2:45][NH:44][C:24]([C:21]1[S:20][C:19]([O:18][C:13]2[CH:14]=[C:15]3[C:10](=[CH:11][CH:12]=2)[O:9][CH:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[CH3:27])[CH2:17][CH2:16]3)=[N:23][CH:22]=1)=[O:25]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 700EthanolamineHCID 6228DimethylformamideHCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 712929842-(2-o-Tolyl-chroman-6-yloxy)-thiazole-5-carboxylic acid lithium salt

Produkt 1

HCID 71509494
2-(2-o-Tolyl-chroman-6-yloxy)-thiazole-5-carboxylic acid (2-hydroxy-ethyl)-amide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 2-(2-o-tolyl-chroman-6-yloxy)-thiazole-5-carboxylic acid lithium salt (100 mg, 0.27 mmol) in dimethylformamide (2 ml) 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (72 mg, 0.38 mmol, 1.4 eq), 1-hydroxy-benzotriazole (51 mg, 0.38 mmol, 1.4 eq) and N-methylmorpholine (68 mg, 0.67 mmol, 2.5 eq) were added and the mixture was stirred at room temperature for 15 min. Ethanolamine (25 mg, 0.40 mmol, 1.5 eq) was added and stirring was continued for 16 h. The mixture was diluted with water and the aqueous layer extracted with ethyl acetate. The combined organic layers were washed with a diluted aqueous solution of sodium carbonate and brine, dried over sodium sulfate and filtered, and the solvent was removed under reduced pressure. The crude product was purified by column chromatography (silica gel, ethyl acetate/methanol gradient). The desired compound was obtained as a white powder (43 mg, 39%).

Aufarbeitung

  1. stirringstirring
  2. waitwas continued for 16 h
  3. extractionthe aqueous layer extracted with ethyl acetate
  4. washThe combined organic layers were washed with a diluted aqueous solution of sodium carbonate and brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customthe solvent was removed under reduced pressure
  8. customThe crude product was purified by column chromatography (silica gel, ethyl acetate/methanol gradient)

Quellen und Nachweise

ORD-Eintrag
ord-413319050c58480c941e0286e89a1c10
Quelldatensatz
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08912224B2

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