Methyl iodide → HCID 67448855, 화합물

HRID 68670노트

반응식

HRID 68670 반응식
[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([SH:17])=[N:7][N:8]2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=1.[C:18]([O-])([O-])=O.[Cs+].[Cs+].IC>CC#N>[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([S:17][CH3:18])=[N:7][N:8]2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 178527921HCID 178527921, 화합물

생성물 1

HCID 67448855HCID 67448855, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Into a 500-mL 3-necked round-bottom flask, was placed a solution of 6-bromo-1-phenyl-1H-indazole-3-thiol (24 g, 78.69 mmol, 1.00 equiv) in CH3CN (200 mL), Cs2CO3 (28.8 g, 88.34 mmol, 1.12 equiv). To the resulting mixture as then added iodomethane (12.6 g, 88.73 mmol, 1.13 equiv) dropwise with stirring at room temperature. The resulting solution was stirred for 60 min at room temperature. The solids were filtered out. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:100) to yield 6-bromo-3-(methylthio)-1-phenyl-1H-indazole as a yellow solid. MS: 328 (MH+).

후처리

  1. customInto a 500-mL 3-necked round-bottom flask, was placed
  2. filtrationThe solids were filtered out
  3. concentrationThe resulting mixture was concentrated under vacuum

출처 및 근거

ORD 기록
ord-e24347ed936b42c58c2bf9e6010016e9
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822447B2

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