Sulfuric Acid → 1-tert-Butyl-5-(2-bromophenyl)-1H-tetrazole
反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[NH:12][N:11]=[N:10][N:9]=1.[CH3:13][C:14](O)([CH3:16])[CH3:15].OS(O)(=O)=O>FC(F)(F)C(O)=O>[C:14]([N:9]1[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Br:1])=[N:12][N:11]=[N:10]1)([CH3:16])([CH3:15])[CH3:13]参加物
5
実験手順
To a solution of 5-(2-bromophenyl)-1H-tetrazole (7.9 g, 0.035 mol) in trifluoroacetic acid (35 mL) was added tBuOH (5.2 g, 0.070 mol) and H2SO4 (1.0 mL, 0.0175 mol). After 18 h, the solution was concentrated and the residue was taken up in EtOAc. The mixture was washed with water, 2.5 N NaOH, water, dried (MgSO4), and concentrated. Purification by flash chromatography (20% EtOAc/hexane) gave 6.6 g (67%) of product as a pale yellow oil.
後処理
- concentrationthe solution was concentrated
- washThe mixture was washed with water, 2.5 N NaOH, water
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customPurification by flash chromatography (20% EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-7a96e231205341d18bf548790214ba78
- 出典データセット
- uspto-grants-1996_03
- 特許番号
- US05498776
反応ノート
読み込み中…