Diethanolamine → 2-Butyl-1,3,6,2-dioxazaborocane
反応式
[NH:1]([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4].[CH2:8]([B:12](O)O)[CH2:9][CH2:10][CH3:11]>C(Cl)Cl.CCOCC>[CH2:8]([B:12]1[O:7][CH2:6][CH2:5][NH:1][CH2:2][CH2:3][O:4]1)[CH2:9][CH2:10][CH3:11]参加物
5
実験手順
To a solution of 2,2′-azanediyldiethanol (26.12 g, 246 mmol) in DCM (250 ml) and ether (500 mL) was added n-butylboronic acid (25.4 g, 242 mmol) and molecular sieves (3 A, 4-6 mesh, 65 g). It was stirred at ambient temperature for 2 hours. The mixture was filtered, and the filtrate was concentrated under reduced pressure. The resulting white solid was recrystallized with DCM/ether to provide white crystals as the title product. NMR (300 MHz, CDCl3): 0.47 (t, J=9 Hz, 2H), 0.88 (t, J=6 Hz, 3H), 1.20-1.37 (m, 4H), 2.82 (br, 2H), 3.24 (br, 2H), 3.95 (br, 4H), 4.27 (br, 1H). MS (DCl—NH3) m/z 172 (M+H)+.
後処理
- filtrationThe mixture was filtered
- concentrationthe filtrate was concentrated under reduced pressure
- customThe resulting white solid was recrystallized with DCM/ether
出典と根拠
- ORDレコード
- ord-db03d468d49e4c58947202e9e95b2d43
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08829041B2
反応ノート
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