Water → HCID 20301865、化合物

HRID 2164038ノート

反応式

HRID 2164038 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-1806ebde1e544dfab62a7370e1df1492
出典データセット
uspto-grants-1979_01
特許番号
US04137310

反応ノート

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