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Ethanolamine → 1-[N-(2-Hydroxyethyl)carbamoyl]-4-[1-[3-(isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzene

HRID 582296
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 582296
[CH:1]([NH:4][C:5]1[C:6]([N:11]2[CH2:16][CH2:15][N:14]([C:17]([C:19]3[CH:27]=[CH:26][C:22]([C:23](O)=[O:24])=[CH:21][CH:20]=3)=[O:18])[CH2:13][CH2:12]2)=[N:7][CH:8]=[CH:9][CH:10]=1)([CH3:3])[CH3:2].C(N(CC)CC)C.C(Cl)(=O)C(C)(C)C.[NH2:42][CH2:43][CH2:44][OH:45]>C(Cl)Cl>[OH:45][CH2:44][CH2:43][NH:42][C:23]([C:22]1[CH:26]=[CH:27][C:19]([C:17]([N:14]2[CH2:15][CH2:16][N:11]([C:6]3[C:5]([NH:4][CH:1]([CH3:2])[CH3:3])=[CH:10][CH:9]=[CH:8][N:7]=3)[CH2:12][CH2:13]2)=[O:18])=[CH:20][CH:21]=1)=[O:24]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 700EthanolamineHCID 8471Triethylamine2×HCID 62493Pivaloyl chlorideHCID 109595584-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoic acid

Produkt 1

HCID 110801221-[N-(2-Hydroxyethyl)carbamoyl]-4-[1-[3-(isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzeneAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

4-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoic acid (1.5 g) was dissolved in methylene chloride (50 ml) and then, triethylamine (0.7 ml) was added and cooled. Pivaloyl chloride(0.58 ml) was added slowly to the solution at 0~5° C. and the mixture was stirred at 5° C. for 2 hours. And then, triethylamine (0.7 ml) and 2-aminoethanol(1.27 g) were added in order, the solution was stirred at 0~5° C. for 2 hours and heated slowly to 20~25° C. and stirred for 30 minutes. The reaction mixture was washed with water twice and the solvent was concentrated under reduced pressure. The concentrated residue was crystallized by treatment with ether and further recrystallized using isopropanol and ether. The recrystallized product was filtered and dried to give 1.34 g (yield: 80%) of the desired compound as a white powder.

Aufarbeitung

  1. temperaturecooled
  2. stirringthe solution was stirred at 0~5° C. for 2 hours
  3. temperatureheated slowly to 20~25° C.
  4. stirringstirred for 30 minutes
  5. washThe reaction mixture was washed with water twice
  6. concentrationthe solvent was concentrated under reduced pressure
  7. customThe concentrated residue was crystallized by treatment with ether
  8. customfurther recrystallized
  9. filtrationThe recrystallized product was filtered
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7fb65c950ed74fbeada699147c6f1b65
Quelldatensatz
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05922871

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