Ethanolamine → HCID 69671185, Verbindung

HRID 626785

Reaktionsgleichung

Reaktionsgleichung von HRID 626785
Cl[C:2]1[N:7]=[C:6]([CH3:8])[N:5]=[C:4]([NH2:9])[CH:3]=1.[CH2:10]([CH2:12][NH2:13])[OH:11].CO>C(OCC)(=O)C>[NH2:9][C:4]1[N:5]=[C:6]([CH3:8])[N:7]=[C:2]([NH:13][CH2:12][CH2:10][OH:11])[CH:3]=1

Komponenten

5

Edukt 3

HCID 700EthanolamineHCID 887MethanolHCID 2867546-Chloro-2-methylpyrimidin-4-amine

Produkt 1

HCID 69671185HCID 69671185, VerbindungAusbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
250 °C

Versuchsvorschrift

A mixture of 6-chloro-2-methylpyrimidin-4-ylamine (717 mg, 5.0 mmol) and ethanolamine (0.602 mL, 10.0 mmol) were heated at 250° C. in a microwave for 30 seconds. After cooling, the residue was dissolved in ethyl acetate, containing a small amount of methanol and was washed with brine. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to afford the title compound as a white solid (334 mg, 40% yield). 1H NMR (400 MHz, DMSO-d6): δ 6.45 (br s, 1H), 5.98 (br s, 2H), 5.25 (s, 1H), 3.47 (t, J=6.0 Hz, 2H), 3.23-3.14 (m, 2H), 2.12 (s, 3H).

Aufarbeitung

  1. temperatureAfter cooling
  2. washwas washed with brine
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6f4aad3310c7482bb8152eb6608ccce9
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09309240B2

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