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Sodium methanethiolate → 6-Methylsulfanyl-[2,2']bipyridin-3-ol

HRID 228803
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HRID 228803 반응식
F[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]([O:14]C)=[CH:4][CH:3]=1.[CH3:16][S-:17].[Na+]>CN(C)C=O>[CH3:16][S:17][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]([OH:14])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4378561Sodium methanethiolateHCID 688295916-Fluoro-3-methoxy-[2,2']bipyridine

생성물 1

HCID 1363851056-Methylsulfanyl-[2,2']bipyridin-3-ol수율 47%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
160 °C

실험 절차

6-Fluoro-3-methoxy-[2,2′]bipyridine (12 mg) and sodium thiomethoxide (41 mg) were suspended in N,N-dimethylformamide (1.5 ml), and the suspension was stirred at 160° C. overnight. The reaction solution was cooled to room temperature, the reaction solution was then filtered, and the solvent was removed from the filtrate by distillation under the reduced pressure. The residue was purified by thin layer chromatography using acetone-chloroform to give 6-methylsulfanyl-[2,2′]bipyridin-3-ol (6 mg, yield 47%).

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후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. filtrationthe reaction solution was then filtered
  3. customthe solvent was removed from the filtrate by distillation under the reduced pressure
  4. customThe residue was purified by thin layer chromatography

출처 및 근거

ORD 기록
ord-fca730f4c80049ef8a80896a37a8cb98
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07560558B2

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