Aluminium lithium hydride → (4-Isopropylpyridin-2-yl)methanamine
反応式
[CH:1]([C:4]1[CH:9]=[CH:8][N:7]=[C:6]([C:10]#[N:11])[CH:5]=1)([CH3:3])[CH3:2].[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH:1]([C:4]1[CH:9]=[CH:8][N:7]=[C:6]([CH2:10][NH2:11])[CH:5]=1)([CH3:3])[CH3:2]参加物
4
実験手順
To a stirring solution of 149 mg (1.01 mmol) of 4-isopropylpicolinonitrile in 7 mL of THF at 0° C. was added 150 mg (3.95 mmol) of LiAlH4. After about 15 min., 250 mg of LiAlH4 was added, and after about 15 min. the ice bath was removed and stirring was continued with warming to r.t. After 40 min., 400 μL of H2O, 400 μL of 15% NaOH (aq), and 1.2 mL of brine were added in succession. The mixture was stirred for 85 min., filtered through Celite, and conc. to give 143 mg of (4-isopropylpyridin-2-yl)methanamine which was used without further purification.
後処理
- customafter about 15 min. the ice bath was removed
- waitAfter 40 min.
- addition400 μL of H2O, 400 μL of 15% NaOH (aq), and 1.2 mL of brine were added in succession
- stirringThe mixture was stirred for 85 min.
- filtrationfiltered through Celite
出典と根拠
- ORDレコード
- ord-c080f00cdb3448cca8d7c3720b23e52e
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08299267B2
反応ノート
読み込み中…