Triethylamine → HCID 67494092, Verbindung

HRID 1968930Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1968930
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:19])=[C:6]([NH:8][C:9](=[O:18])/[CH:10]=[CH:11]/[C:12]2[CH:17]=[CH:16][CH:15]=CN=2)[CH:7]=1.[CH2:20]([N:22](CC)CC)C.[CH3:27][C:28]1[CH:36]=[CH:35][C:31]([C:32](Cl)=[O:33])=[CH:30][CH:29]=1.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH3:19][C:5]1[CH:4]=[CH:3][C:2]([NH:1][C:32](=[O:33])[C:31]2[CH:35]=[CH:36][C:28]([CH3:27])=[CH:29][CH:30]=2)=[CH:7][C:6]=1[NH:8][C:9](=[O:18])[CH:10]=[CH:11][C:12]1[CH:20]=[N:22][CH:15]=[CH:16][CH:17]=1

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 134054-Methylbenzoyl ChlorideHCID 86664945HCID 86664945, Verbindung

Produkt 1

HCID 67494092HCID 67494092, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of the product of step 3 (0.25 g) and triethylamine (0.2 ml) in dichloromethane (25 ml), a solution of 4-methylbenzoyl chloride (0.5 g) in dichloromethane (10 ml) was added dropwise slowly in an ice-bath with the temperature no more than 5° C. After addition, the reaction was carried out for to 30 min in an ice-bath, and then at room temperature overnight. The completion of reaction was indicated by TLC. After that potassium carbonate solution (10%) was added, and then a solid was precipitated, and filtered out. The filter cake was washed with water, and recrystallized from ethyl acetate to give a solid.

Aufarbeitung

  1. additionAfter addition
  2. customthe reaction was carried out for to 30 min in an ice-bath
  3. customat room temperature
  4. customovernight
  5. customThe completion of reaction
  6. customa solid was precipitated
  7. filtrationfiltered out
  8. washThe filter cake was washed with water
  9. customrecrystallized from ethyl acetate
  10. customto give a solid

Quellen und Nachweise

ORD-Eintrag
ord-eedb9b2f82144a73bfd75213a84c032e
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08426446B2

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