Sulfuric Acid → 2-Chloro-6-fluoroaniline

HRID 437954

반응식

HRID 437954 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1C(O)=O.S(=O)(=O)(O)O.[N-:17]=[N+]=[N-].[Na+].[OH-].[Na+]>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[NH2:17]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 33557Sodium AzideHCID 679472-Chloro-6-fluorobenzoic acid

생성물 1

HCID 27342052-Chloro-6-fluoroaniline

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a stirred mixture of 20 g. of 2-chloro-6-fluorobenzoic acid, 100 ml. of chloroform and 50 ml. of concentrated sulfuric acid is added slowly 10.2 g. of sodium azide while the temperature is kept at 40°-55°. Stirring is continued for 2 hours at 40°-55° then the mixture is poured into 500 ml. of ice water containing 80 g. of sodium hydroxide. The mixture is extracted with ether and the other extracts are dried over magnesium sulfate. The dry extracts are then treated with hydrogen chloride, and the resultant product as the hydrochloride salt is collected by filtration yielding 12.6 g. of white solid which sublimes at 160°-170°.

후처리

  1. additionTo a stirred mixture of 20 g
  2. customis kept at 40°-55°
  3. additionthe mixture is poured into 500 ml
  4. extractionThe mixture is extracted with ether
  5. dry with materialthe other extracts are dried over magnesium sulfate
  6. additionThe dry extracts are then treated with hydrogen chloride
  7. filtrationthe resultant product as the hydrochloride salt is collected by filtration
  8. customyielding 12.6 g
  9. customsublimes at 160°-170°

출처 및 근거

ORD 기록
ord-3e0bfc85cb5844a6a56847ee7894b893
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04032639

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