Water → HCID 20301865, 화합물

HRID 2164038노트

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HRID 2164038 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 20301865HCID 20301865, 화합물수율 53.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1806ebde1e544dfab62a7370e1df1492
출처 데이터셋
uspto-grants-1979_01
특허 번호
US04137310

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