6-Bromo-N-(tert-butyl)-3-methylpyridin-2-amine → 6-Bromo-3-methylpyridin-2-amine
反応式
[Br:1][C:2]1[N:7]=[C:6]([NH:8]C(C)(C)C)[C:5]([CH3:13])=[CH:4][CH:3]=1>ClCCCl.C(O)(C(F)(F)F)=O>[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH3:13])=[CH:4][CH:3]=1参加物
4
実験手順
A solution of (6-bromo-3-methylpyridin-2-yl)-tert-butylamine (500 mg, 2.06 mmol) in DCE (2 mL) and TFA (2 mL) was heated at 120° C. for 10 min in a microwave reactor, and then concentrated under reduced pressure. The residue was taken up in MeOH and loaded onto an Isolute® SCX-2 cartridge (10 g). The cartridge was washed with MeOH then the desired product eluted with 2 M NH3 in MeOH to give 6-Bromo-3-methylpyridin-2-ylamine as a white solid (359 mg, 93%). 1H NMR (400 MHz, CHCl3-d): δ 7.11 (d, J=7.5 Hz, 1 H); 6.77 (d, J=7.5 Hz, 1 H); 4.50 (s, 2 H); 2.07 (s, 3 H).
後処理
- concentrationconcentrated under reduced pressure
- washThe cartridge was washed with MeOH
- washthe desired product eluted with 2 M NH3 in MeOH
出典と根拠
- ORDレコード
- ord-9d1397765ded4f91b9e01a30b2dabc50
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08173650B2
反応ノート
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