Sulfuric Acid → 2-Chloro-6-fluoroaniline

HRID 372202ノート

反応式

HRID 372202 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 27342052-Chloro-6-fluoroaniline

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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°.

後処理

  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°

出典と根拠

ORDレコード
ord-5d57431d5123479d821730b42fd73031
出典データセット
uspto-grants-1978_05
特許番号
US04089958

反応ノート

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