5-Fluoro-2-nitroanisole → (3-methoxy-4-nitrophenyl)(methyl)sulfane(WX191877)

HRID 2283508ノート

反応式

HRID 2283508 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([O:11][CH3:12])[CH:3]=1.[CH3:13][S-:14].[Na+]>CN(C=O)C.O>[CH3:12][O:11][C:4]1[CH:3]=[C:2]([S:14][CH3:13])[CH:7]=[CH:6][C:5]=1[N+:8]([O-:10])=[O:9]

参加物

5

反応物 2

HCID 27792505-Fluoro-2-nitroanisoleHCID 4378561Sodium methanethiolate

生成物 1

HCID 86688022(3-methoxy-4-nitrophenyl)(methyl)sulfane(WX191877)収率 59.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 4-fluoro-2-methoxy-1-nitrobenzene (1.38 g, 8.06 mmol) and sodium methyl mercaptide (0.622 g, 8.87 mmol) in DMF (25 mL) was stirred at room temperature for 18 hours. The reaction was the diluted with water and extracted with EtOAc. The combined extracts were washed with brine, dried over sodium sulfate, filtered and concentrated to give (3-methoxy-4-nitrophenyl)(methyl)sulfane (0.95 g, 59%).

後処理

  1. extractionextracted with EtOAc
  2. washThe combined extracts were washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-86ecef930b4c4432b501cd96b42cc925
出典データセット
uspto-grants-2015_09
特許番号
US09145402B2

反応ノート

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