Reaktion #9821

Reaktionsgleichung

methyl magnesium bromide

4-Methylamino-2-methylsulfanyl-pyrimidine-5-carbaldehyde

→

1-(4-Methylamino-2-methylsulfanyl-pyrimidin-5-yl)-ethanol

Lösungsmittel

ether

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONanother 14 ml Grignard solution were added within 30 min
2. 2
   workup.STIRRINGStirring
3. 3
   workup.WAITwas continued for 30 min at 0° C. and finally at RT for 25 hrs
4. 4
   SonstigeThe mixture was quenched with saturated ammonium chloride solution
5. 5
   Extraktionextracted with ethyl acetate

Vorschrift

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.

Quelle