Bromine → 6-Amino-7-bromobenzothiazole
反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]2[N:6]=[CH:7][S:8][C:4]=2[CH:3]=1.[Br:11]Br.CCOC(C)=O.CCCCCC>CC(O)=O.CCOC(C)=O>[Br:11][C:3]1[C:4]2[S:8][CH:7]=[N:6][C:5]=2[CH:9]=[CH:10][C:2]=1[NH2:1]参加物
6
反応条件
- 温度
- 25 °C
実験手順
To a solution of 6-aminobenzothiazole (16 g, 107 mmol) in 100 mL of AcOH was added Br2 (2.0 mL, 43 mmol) dropwise and the resulting reaction mixture was stirred for 1 h at 25° C. Reaction mixture was concentrated in vacuo, yielding a yellow solid which was dissolved in EtOAc and washed with aq. NaHCO3. Organic layer was dried over Na2SO4 and concentrated in vacuo, yielding an oil which was subjected to column chromatography (10-50% EtOAc/n-Hexane) to obtain 7.8 g (34 mmol, 80% ) of the desired product.
後処理
- customthe resulting reaction mixture
- customReaction mixture
- concentrationwas concentrated in vacuo
- customyielding a yellow solid which
- washwashed with aq. NaHCO3
- dry with materialOrganic layer was dried over Na2SO4
- concentrationconcentrated in vacuo
- customyielding an oil which
出典と根拠
- ORDレコード
- ord-88a5e7a6c99342baa3100ee7104fb62c
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06303643B1
反応ノート
読み込み中…