反応 #1331511

ord-7ac00c810eb248628cf6dc33e3e531e7

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction mixture was concentrated
  2. 2
    その他adjusted to pH 10 with ammonium hydroxide (25%), whereupon a precipitation
  3. 3
    その他formed
  4. 4
    その他The precipitation
  5. 5
    ろ過was filtered
  6. 6
    洗浄the crystals washed with water
  7. 7
    その他After drying in vacuo

実験手順

0.03 g [3-Methoxymethyl-2-(4-methoxy-7-morpholin-4-yl-benzothiazol-2-yl)-3H-imidazo[4,5-b]pyridin-5-yl]-methyl-(tetrahydro-pyran-4-ylmethyl)-amine (0.056 mmol) were treated with 5N HCl (1 ml) at 90° C. for 0.5 h. The reaction mixture was concentrated, taken up in water (1 ml) and adjusted to pH 10 with ammonium hydroxide (25%), whereupon a precipitation formed. The precipitation was filtered, the crystals washed with water. After drying in vacuo, 0.015 g [2-(4-methoxy-7-morpholin-4-yl-benzothiazol-2-yl)-3H-imidazo[4,5-b]pyridin-5-yl]-methyl-(tetrahydro-pyran-4-ylmethyl)-amine (55%) was obtained as a yellow solid; M.p.: 190–195° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07122545B2uspto-grants-2006_10