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Methyl iodide → 7-Bromo-2-methylsulfanyl-1,3-benzothiazole

HRID 389577
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HRID 389577 반응식
C(=O)([O-])[O-].[K+].[K+].[Br:7][C:8]1[C:16]2[S:15][C:14](=[S:17])[NH:13][C:12]=2[CH:11]=[CH:10][CH:9]=1.CI.[CH3:20]COC(C)=O>CN(C=O)C>[Br:7][C:8]1[C:16]2[S:15][C:14]([S:17][CH3:20])=[N:13][C:12]=2[CH:11]=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 118507717-Bromobenzo[D]thiazole-2-thiol

생성물 1

HCID 667606187-Bromo-2-methylsulfanyl-1,3-benzothiazole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

Potassium carbonate (67 mg, 0.49 mmol) was added to a solution of 7-bromo-1,3-benzothiazole-2(3H)-thione (100 mg, 0.41 mmol) in DMF (5 mL). The mixture was stirred at room temperature for 30 min. Methyl iodide (25 μL, 0.41 mmol) was added and the resulting mixture was stirred at room temperature for 30 min. EtOAc was added the separated organic fraction was washed with water and brine, dried over sodium sulfate, and concentrated. The title compound thus obtained was used without further purification. MS (ESI): 260.34, 262.32 [M+H]+; HPLC tR=1.54 min (HPLC: Anayltical—2 min).

후처리

  1. stirringthe resulting mixture was stirred at room temperature for 30 min
  2. washwas washed with water and brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3c50b97598664657871d1c3bcc18f2be
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08378104B2

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