1,4-Dibromobutane → HCID 68630196, 화합물
반응식
[S:1]1[C:5]2[CH:6]=[CH:7][C:8]([OH:10])=[CH:9][C:4]=2[N:3]=[CH:2]1.[Br:11][CH2:12][CH2:13][CH2:14][CH2:15]Br.C([O-])([O-])=O.[K+].[K+]>CCO>[Br:11][CH2:12][CH2:13][CH2:14][CH2:15][O:10][C:8]1[CH:7]=[CH:6][C:5]2[S:1][CH:2]=[N:3][C:4]=2[CH:9]=1참가 물질
5
실험 절차
A mixture of intermediate 25 (206 mg, 1.4 mmol), 1,4-dibromobutane (0.5 mL, 4.2 mmol) and anhydrous K2CO3 (193 mg, 1.4 mmol) in EtOH (20 mL) was heated to reflux and stirred overnight. The yellow solid was filtered and purified by column chromatography (elution with PE/EtOAc=4:1) to afford 5-(4-bromobutoxy)benzo[d]thiazole (intermediate 26) (108 mg, 39%) as a yellow oil. HPLC: 99%, RT 3.426 min. MS (ESI) m/z 288.0 [M+H]+.
후처리
- temperaturewas heated
- temperatureto reflux
- filtrationThe yellow solid was filtered
- custompurified by column chromatography (elution with PE/EtOAc=4:1)
출처 및 근거
- ORD 기록
- ord-a02c0d8cf99e480684f93acaaf04fb81
- 출처 데이터셋
- uspto-grants-2015_10
- 특허 번호
- US09156822B2
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