4-(Methylamino)-2-(methylthio)pyrimidine-5-carbaldehyde → 1-(4-Methylamino-2-methylsulfanyl-pyrimidin-5-yl)-ethanol

HRID 9725Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 9725
[CH3:1][NH:2][C:3]1[C:8]([CH:9]=[O:10])=[CH:7][N:6]=[C:5]([S:11][CH3:12])[N:4]=1.[CH3:13][Mg]Br>C1COCC1.CCOCC>[CH3:1][NH:2][C:3]1[C:8]([CH:9]([OH:10])[CH3:13])=[CH:7][N:6]=[C:5]([S:11][CH3:12])[N:4]=1

Komponenten

5

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

1.5 g 4-Methylamino-2-methylsulfanyl-pyrimidine-5-carbaldehyde were dissolved in 30 ml THF and 14 ml of a 1.4 M solution of methyl magnesium bromide in ether were added dropwise below 5° C. After stirring for 1 hr at 0° C., another 14 ml Grignard solution were added within 30 min. Stirring was continued for 30 min at 0° C. and finally at RT for 25 hrs. The mixture was quenched with saturated ammonium chloride solution and extracted with ethyl acetate.

Aufarbeitung

  1. additionanother 14 ml Grignard solution were added within 30 min
  2. stirringStirring
  3. waitwas continued for 30 min at 0° C. and finally at RT for 25 hrs
  4. customThe mixture was quenched with saturated ammonium chloride solution
  5. extractionextracted with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-c30e63ee47dc475e94aad2aa23ea7648
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07091345B2

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