反応 #1265391

ord-65f54278019f4e40ba4d907565301998

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool
  2. 2
    濃縮concentrated under high vacuum to an oil
  3. 3
    その他The residue was purified by HPLC with 0.1% TFA/water acetonitrile as eluant

実験手順

To solution of [4-(5-Chloro-thiazol-2-yl)-pyrimidin-2-yl]-(3,4,5-trimethoxy-phenyl)-amine (150 mg) in dimethylsulfoxide (2 ml) was added piperazine (300 mg). The mixture was heated to 100° C. for 5 hours then allowed to cool and concentrated under high vacuum to an oil. The residue was purified by HPLC with 0.1% TFA/water acetonitrile as eluant to afford the sub-titled compound as an yellow solid (40 mg, 25%); IR (solid) 1567, 1504, 1432, 1411 cm−1; 1H NMR (400 Mhz, CDCl3) δ 1.3-1.5 (1H, br s), 3.1 (4H, s), 3.25 (4H, s), 3.85 (3H, s), 3.95 (6H, s), 7.05 (1H, s), 7.15 (1H, s), 7.19 (1H, s), 7.40 (1H, m), 8.6 (1H, d); MS (ES+) 429.3 (M+1), (ES−) 427.3 (M−1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07276502B2uspto-grants-2007_10