Bromine → 5,7-Difluorobenzo[d]thiazol-2-amine
反応式
[F:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]([NH2:12])=[S:11])[CH:5]=[C:6]([F:8])[CH:7]=1.BrBr>ClCCCl>[F:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]2[S:11][C:10]([NH2:12])=[N:9][C:4]=2[CH:3]=1参加物
4
反応条件
- 温度
- 10 °C
実験手順
To a suspension of N-(3,5-difluorophenyl) thiourea (3.40 g, 18.07 mmol) in DCE (95 mL) was added a solution of bromine in DCE (5 mL) below 30° C. The mixture was heated at reflux for 2.5 h, then cooled to 10° C., and the precipitate formed was collected by filtration and washed with DCE. The solid was stirred with water (200 mL), basified by treatment with conc. ammonium hydroxide, filtered, and dried in a vacuum oven to afford 5,7-difluoro-1,3-benzothiazol-2-amine (3.05 g, 90%). ret. time 2.18; m/z 187.1 (NH+); 1H NMR (400 MHz, DMSO-d6) δ 6.92 (m, 1H), 7.00 (m, 2H), 7.92 (s, 2H).
後処理
- temperatureThe mixture was heated
- temperatureat reflux for 2.5 h
- customthe precipitate formed
- filtrationwas collected by filtration
- washwashed with DCE
- filtrationfiltered
- customdried in a vacuum oven
出典と根拠
- ORDレコード
- ord-4f7aa1f4483046469aab193d0211f406
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091228B2
反応ノート
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