反応 #10008

ord-65634670e10c47c68865d9e95be13558

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool
  2. 2
    洗浄The organic phase is washed with water
  3. 3
    その他separated off
  4. 4
    乾燥dried over sodium sulfate
  5. 5
    濃縮On concentration

実験手順

0.2 g (0.62 mmol) of 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine (prepared according to Stage 90.2) is stirred in 1 ml of ethanolamine at 150° C. for 3 h, and the mixture is allowed to cool and is diluted with ethyl acetate. The organic phase is washed with water, separated off and dried over sodium sulfate. On concentration, 2-(2-hydroxy-ethyl-amino)-6-(3-fluoro-phenyl-amino)-9-ethyl-9H-purine is obtained as a crystalline precipitate. This precipitate is filtered off and dried; m.p. 184° C.; FAB-MS: (M+H)+=317; Rf=0.5 (CH2Cl2:methanol=9:1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091346B1uspto-grants-2006_08