Dichloromethane → HCID 117824150、化合物

HRID 59102

反応式

HRID 59102 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[O:11][CH3:12].[CH3:13][O:14][C:15]1[N:16]=[CH:17][NH:18][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].C(Cl)Cl>C(#N)C>[CH3:13][O:14][C:15]1[N:16]=[CH:17][N:18]([C:2]2[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=2[O:11][CH3:12])[CH:19]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 144519681-Fluoro-2-methoxy-4-nitrobenzeneHCID 178493803HCID 178493803、化合物

生成物 1

HCID 117824150HCID 117824150、化合物収率 54.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
90 °C

実験手順

1-Fluoro-2-methoxy-4-nitrobenzene (0.785 g, 4.59 mmol), 4-methoxy-1H-imidazole (0.45 g, 4.59 mmol) and potassium carbonate (0.697 g, 5.05 mmol) were mixed in dry acetonitrile (10 mL) and heated at 90° C. for 4 days. DCM was added and the mixture was filtrated through a pad of silica eluting with 5% MeOH in DCM. The solvents were evaporated and mixture was purified by column chromatography in silica eluting with a gradient of MeOH and DCM to give the title compound as a gum 0.62 g (54%).

後処理

  1. filtrationthe mixture was filtrated through a pad of silica eluting with 5% MeOH in DCM
  2. customThe solvents were evaporated
  3. custommixture was purified by column chromatography in silica eluting with a gradient of MeOH and DCM

出典と根拠

ORDレコード
ord-fdfba193e4ce4de8bd37a02c85fe590f
出典データセット
uspto-grants-2016_09
特許番号
US09439904B2

関連ノート

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