Water → HCID 22136372, Verbindung

HRID 1826874Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1826874
Cl.[N:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12](Cl)=[O:13])=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1.[C:15]12([OH:25])[CH2:24][CH:19]3[CH2:20][CH:21]([CH2:23][CH:17]([CH2:18]3)[CH2:16]1)[CH2:22]2.O>N1C=CC=CC=1>[N:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]([O:25][C:15]34[CH2:22][CH:21]5[CH2:20][CH:19]([CH2:18][CH:17]([CH2:23]5)[CH2:16]3)[CH2:24]4)=[O:13])=[CH:9][CH:10]=2)[CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 641521-AdamantanolHCID 22136358Quinoline-6-carbonyl chloride hydrochloride

Produkt 1

HCID 22136372HCID 22136372, VerbindungAusbeute 31,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel2×

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

6-Quinolinecarbonyl chloride hydrochloride (0.76 g, 3.3 mmol) in pyridine (2 mL) was added to a solution of 1-adamantanol (0.60 g, 3.9 mmol) in pyridine (8 mL). The reaction was stirred at 70° C. for 16 h. To the stirring reaction mixture was added water (100 mL) which caused the product to precipitate. This precipitate was filtered and then washed with water (3×25 mL). The filter cake was dissolved in ethanol (20 mL) and water was then added to the cloud point (16 mL). The crystallizing solution was allowed to stand for 15 h. Filtering and drying under high vacuum for 7 h provided 0.32 g (26%) of (61) as light brown needle-like crystals:

Aufarbeitung

  1. customTo the stirring reaction mixture
  2. customto precipitate
  3. filtrationThis precipitate was filtered
  4. washwashed with water (3×25 mL)
  5. dissolutionThe filter cake was dissolved in ethanol (20 mL)
  6. additionwater was then added to the cloud point (16 mL)
  7. waitto stand for 15 h
  8. filtrationFiltering
  9. customdrying under high vacuum for 7 h

Quellen und Nachweise

ORD-Eintrag
ord-96bee3001af4484ca83846fc6cd86274
Quelldatensatz
uspto-grants-2006_05
Patentnummer
US07053104B2

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