Water → HCID 20301865、化合物

HRID 1732869ノート

反応式

HRID 1732869 の反応式
[Cl:1][C:2]1[C:8](Cl)=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=[CH:5][C:3]=1[NH2:4].[CH3:13][O-:14].[Na+].O>CO>[Cl:1][C:2]1[C:8]([O:14][CH3:13])=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=[CH:5][C:3]=1[NH2:4]

参加物

5

反応物 3

HCID 962WaterHCID 30139982,3-dichloro-4-nitroanilineHCID 10942334Sodium Methoxide

生成物 1

HCID 20301865HCID 20301865、化合物収率 53.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2,3-dichloro-4-nitroaniline (25 g) and sodium methoxide (25 g) in methanol (250 ml) is stirred and heated at reflux under a nitrogen atmosphere for 5.5 hours. The reaction mixture is poured into water (1.5 l), the precipitated yellow solid is collected and dried. This material is purified by chromatography on silica gel using 1:1 hexane/ether eluent. The eluents are collected and evaporated to dryness to afford 13 g of title compound, m.p. 118°-123° C.

後処理

  1. temperatureheated
  2. temperatureat reflux under a nitrogen atmosphere for 5.5 hours
  3. customthe precipitated yellow solid is collected
  4. customdried
  5. customThis material is purified by chromatography on silica gel using 1:1 hexane/ether eluent
  6. customThe eluents are collected
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-6421c56451444848914f136bc6cca713
出典データセット
uspto-grants-1980_12
特許番号
US04239708

反応ノート

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