Methyl iodide → HCID 67448855、化合物

HRID 68670ノート

反応式

HRID 68670 の反応式
[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

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 178527921HCID 178527921、化合物

生成物 1

HCID 67448855HCID 67448855、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-e24347ed936b42c58c2bf9e6010016e9
出典データセット
uspto-grants-2014_09
特許番号
US08822447B2

反応ノート

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