反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH2:11][C:12]1[NH:13][CH2:14][CH2:15][N:16]=1)[CH:6]=[C:5]2[S:17]([CH2:20][CH2:21][O:22]C1CCCCO1)(=[O:19])=[O:18]>C(O)(=O)C.O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH2:11][C:12]1[NH:13][CH2:14][CH2:15][N:16]=1)[CH:6]=[C:5]2[S:17]([CH2:20][CH2:21][OH:22])(=[O:18])=[O:19]参加物
3
反応条件
- 温度
- 47.5 °C
実験手順
The 5-chloro-1-(4,5-dihydro-1H-imidazol-2-ylmethyl)-3-[2-(tetrahydro-pyran-2-yloxy)-ethanesulfonyl]-1H-indole (0.028 g) prepared in the previous Step was dissolved in 4 ml acetic acid:water (2:1) and stirred at 45-50° C. for 3 h. The solvents were removed under reduced pressure and the crude product was purified by column chromatography (silica gel) eluting with 3-5% methanol in methylene chloride with 0.1% ammonium hydroxide added. The 2-[5-Chloro-1-(4,5-dihydro-1H-imidazol-2-ylmethyl)-1H-indole-3-sulfonyl]-ethanol thus obtained weighed 0.005 g after drying.
後処理
- customThe solvents were removed under reduced pressure
- customthe crude product was purified by column chromatography (silica gel)
- washeluting with 3-5% methanol in methylene chloride with 0.1% ammonium hydroxide
- additionadded
出典と根拠
- ORDレコード
- ord-99f5b152a87f44f1b7471a0d3254f0ff
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852726B2
関連ノート
読み込み中…