Diisopropylethylamine → HCID 86659399, Verbindung

HRID 2043444Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2043444
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([NH:9][C@H:10]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH3:11])[N:3]=1.Cl.[OH:20][CH2:21][C:22]1([OH:28])[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1.C(N(CC)C(C)C)(C)C>C(OCCO)C.C(OCC)(=O)C>[Cl:8][C:6]1[N:5]=[C:4]([NH:9][C@H:10]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH3:11])[N:3]=[C:2]([N:25]2[CH2:26][CH2:27][C:22]([CH2:21][OH:20])([OH:28])[CH2:23][CH2:24]2)[CH:7]=1

Komponenten

6

Edukt 3

HCID 81531DiisopropylethylamineHCID 227444724-(Hydroxymethyl)-4-piperidinol hydrochlorideHCID 86659372(S)-4,6-Dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidin-2-amine

Produkt 1

HCID 86659399HCID 86659399, VerbindungAusbeute 97,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8076Glycol monoethyl etherLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
135 °C

Versuchsvorschrift

150 mg of (S)-4,6-dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidine-2-amine and 97 mg of 4-(hydroxymethyl)piperidin-4-ol hydrochloride were dissolved in 3 ml of 2-ethoxyethanol, and 274 μl of N,N-diisopropylethylamine was added thereto, and the mixture was stirred at 135° C. for 20 hours. The reaction solution was air-cooled to room temperature, and then diluted with ethyl acetate. The solution was washed in turn with water and brine and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 194 mg of the objective compound as brown oil.

Aufarbeitung

  1. temperatureThe reaction solution was air-cooled to room temperature
  2. washThe solution was washed in turn with water and brine
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6a53b8b3e66042bf81f7f834a4fa0c41
Quelldatensatz
uspto-grants-2013_11
Patentnummer
US08586591B2

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