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Diisopropylethylamine → HCID 21258204, Verbindung

HRID 635218
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 635218
[C:1]1([C:7]2[CH2:12][N:11]([C:13]3[CH:18]=[C:17]([CH3:19])[N:16]=[C:15](Cl)[N:14]=3)[CH2:10][CH2:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[Br:22][C:23]1[CH:29]=[C:28]([CH:30]([CH3:32])[CH3:31])[CH:27]=[CH:26][C:24]=1[NH2:25].C(N(C(C)C)CC)(C)C.C(=O)([O-])O.[Na+]>C(O)CO>[Br:22][C:23]1[CH:29]=[C:28]([CH:30]([CH3:31])[CH3:32])[CH:27]=[CH:26][C:24]=1[NH:25][C:15]1[N:14]=[C:13]([N:11]2[CH2:12][C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)=[CH:8][CH2:9][CH2:10]2)[CH:18]=[C:17]([CH3:19])[N:16]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 21258202HCID 21258202, VerbindungHCID 212582072-Bromo-4-isopropylaniline hydrochloride

Produkt 1

HCID 21258204HCID 21258204, VerbindungAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 174
Ethylene Glycol
Lösungsmittel

Versuchsvorschrift

4-(5-Phenyl-1,2,3,6-tetrahydropyridin-1-yl)-2-chloro-6-methylpyrimidine (1.10 g), 2-bromo-4-isopropylaniline hydrochloride (0.97 g), and diisopropylethylamine (0.50 g) were heated at reflux in 5 ml of ethylene glycol for 1 hour. The reaction solution was poured into a saturated sodium hydrogencarbonate aqueous solution and extracted with ethyl acetate. The extract was washed with water and then with a saturated sodium chloride aqueous solution, and dried over anhydrous sodium sulfate. The desiccant was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate=3/1) to give 1.32 g of 2-[N-(2-bromo-4-isopropylphenyl)amino]-4-(5-phenyl-1,2,3,6-tetrahydropyridin-1-yl)-6-methylpyrimidine as an amorphous substance.

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialwith a saturated sodium chloride aqueous solution, and dried over anhydrous sodium sulfate
  4. filtrationThe desiccant was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate=3/1)

Quellen und Nachweise

ORD-Eintrag
ord-fac391b0fad84f0ab30021cbf62918de
Quelldatensatz
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06187781B1

Notizen zur Reaktion

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