Bromine → 5,7-Difluorobenzo[d]thiazol-2-amine
반응식
[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]=1참가 물질
4
반응 조건
- 온도
- 10 °C
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-4f7aa1f4483046469aab193d0211f406
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091228B2
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