Sodium Hydroxide → 6-Bromoisoquinolin-3-Amine
反応式
[Br:1][C:2]1[CH:18]=[CH:17][C:5]([CH2:6][NH:7][C:8](=[NH:16])[CH:9](OCC)OCC)=[CH:4][CH:3]=1.[OH-].[Na+]>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:18]=[C:17]2[C:5](=[CH:4][CH:3]=1)[CH:6]=[N:7][C:8]([NH2:16])=[CH:9]2参加物
4
実験手順
N-(4-bromobenzyl)-2,2-diethoxyacetimidamide (1.53 g, 4.85 mmol) in sulfuric acid (4 mL, 95-98%) was heated at 40 C for 14 h. The mixture was neutralized with 1 M NaOH to pH 7 and the resulting suspension was filtered. The residue was purified by silica gel chromatography with 20-55% ethyl acetate in hexanes. The desired fractions were concentrated to give a brownish yellow solid (0.434 g, 40%). LCMS: R.T.=1.62; [M+2]+=225.1.
後処理
- filtrationthe resulting suspension was filtered
- customThe residue was purified by silica gel chromatography with 20-55% ethyl acetate in hexanes
- concentrationThe desired fractions were concentrated
出典と根拠
- ORDレコード
- ord-0f59cfa750e14c869e029175ea806df5
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08309577B2
反応ノート
読み込み中…