反応 #9821

ord-c30e63ee47dc475e94aad2aa23ea7648

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  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
    その他The mixture was quenched with saturated ammonium chloride solution
  5. 5
    抽出extracted with ethyl acetate

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091345B2uspto-grants-2006_08