Chloroform → Methyl 4-amino-3,5-dichlorobenzoate

HRID 1441041

반응식

HRID 1441041 반응식
[NH2:1][C:2]1C=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.S(Cl)([Cl:15])(=O)=O.[OH-].[Na+].[CH:19]([Cl:22])(Cl)Cl>>[NH2:1][C:2]1[C:3]([Cl:15])=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][C:19]=1[Cl:22]

참가 물질

5

반응물 4

HCID 6212ChloroformHCID 12082Methyl 4-aminobenzoateHCID 14798Sodium HydroxideHCID 24648Sulfuryl chloride2회

생성물 1

HCID 604808Methyl 4-amino-3,5-dichlorobenzoate

실험 절차

Methyl 4-aminobenzoate (25 g.) in dry chloroform (250 ml.) was treated dropwise with sulphuryl chloride (10 ml.) and the mixture heated at reflux for 4 hours. A further supply of sulphuryl chloride (10 ml.) was added and heating continued for a further 2 hours. The reaction mixture was poured onto ice and 2N sodium hydroxide solution was added. The organic solution was separated and the aqueous phase extracted with ethyl acetate. The combined organic solution was dried (anhydrous magnesium sulphate) and evaporated to give methyl 4-amino-3,5-dichlorobenzoate as a solid.

후처리

  1. temperaturethe mixture heated
  2. temperatureat reflux for 4 hours
  3. temperatureheating
  4. additionwas added
  5. customThe organic solution was separated
  6. extractionthe aqueous phase extracted with ethyl acetate
  7. dry with materialThe combined organic solution was dried (anhydrous magnesium sulphate)
  8. customevaporated

출처 및 근거

ORD 기록
ord-d5b8192b3b144b0399836676248d826a
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05502073

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