Sodium Hydroxide → (2-methyl-6-nitro-2H-indazol-3-yl)methanol
反応式
Br[CH2:2][C:3]1[N:4]([CH3:15])[N:5]=[C:6]2[C:11]=1[CH:10]=[CH:9][C:8]([N+:12]([O-:14])=[O:13])=[CH:7]2.[OH-:16].[Na+]>CC#N.O>[CH3:15][N:4]1[C:3]([CH2:2][OH:16])=[C:11]2[C:6]([CH:7]=[C:8]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:10]2)=[N:5]1参加物
5
実験手順
3-(Bromomethyl)-2-methyl-6-nitro-2H-indazole (4.20 g, ˜14.9 mmol) in CH3CN (500 ml) and water (200 ml) was treated with NaOH to give pH˜11. The solution was stirred at rt for 2 days then conc. in vacuo and repeatedly extracted with dichloromethane and chloroform. The combined organic extracts were evaporated, and the crude product was purified by silica gel column chromatography to give (2-methyl-6-nitro-2H-indazol-3-yl)methanol (1.03 g, 33% TY). MS (ES+, m/z) 208.
後処理
- customto give pH˜11
- extractionconc. in vacuo and repeatedly extracted with dichloromethane and chloroform
- customThe combined organic extracts were evaporated
- customthe crude product was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-e9bc7907d3f64491a47e0ec6e422c76d
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07858626B2
反応ノート
読み込み中…