Triethylamine → N-(3-bromopropyl)acetoacetamide
反応式
[CH2:1]=[C:2]1[O:6][C:4](=[O:5])[CH2:3]1.Br.[Br:8][CH2:9][CH2:10][CH2:11][NH2:12].C(N(CC)CC)C>C1COCC1>[Br:8][CH2:9][CH2:10][CH2:11][NH:12][C:4](=[O:5])[CH2:3][C:2]([CH3:1])=[O:6]参加物
5
実験手順
Diketene (1.22 mL, 15.7 mmol, 1.50 equiv) was added at room temperature to a stirred mixture of 3-bromopropylamine hydrobromide (2.30 g, 10.5 mmol, 1.00 equiv) and triethylamine (1.46 mL, 10.5 mmol, 1.00 equiv) in anhydrous THF (20 mL) under argon, and stirring was continued at room temperature for 1 hour. The solvent was removed and the residue was purified by flash chromatography (SiO2, MeOH—CH2Cl2 0:1 to 1:18) to afford a light yellow oil, 2.10 g (90%), which was characterized spectroscopically.
後処理
- customThe solvent was removed
- customthe residue was purified by flash chromatography (SiO2, MeOH—CH2Cl2 0:1 to 1:18)
- customto afford a light yellow oil, 2.10 g (90%), which
出典と根拠
- ORDレコード
- ord-ab1d04208ba942d5ab38c7f9319c154c
- 出典データセット
- uspto-grants-2001_04
- 特許番号
- US06211198B1
反応ノート
読み込み中…