Hydrochloric Acid → 1-Chloro-3-fluoro-2-nitrobenzene

HRID 437955ノート

反応式

HRID 437955 の反応式
Cl.[Cl:2][C:3]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:4]=1N.Cl.[N:12]([O-:14])=[O:13].[Na+].S([O-])([O-])=O>O>[Cl:2][C:3]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:4]=1[N+:12]([O-:14])=[O:13]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1099SulfiteHCID 203786572-Chloro-6-fluoroaniline hydrochlorideHCID 23668193Sodium Nitrite2 回

生成物 1

HCID 30175001-Chloro-3-fluoro-2-nitrobenzene

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

実験手順

To a solution of 17.2 g. of 2-chloro-6-fluoroaniline hydrochloride and 12.5 ml. of concentrated hydrochloric acid in 150 ml. of water is added slowly a solution of 9 g. of sodium nitrite in 25 ml. of water. The temperature of the solution is kept below 5° at all times. This solution is then added to a stirred suspension of 18 g. of cuprocupric sulfite and 60 g. of sodium nitrite in 300 ml. of water at room temperature. The mixture is stirred for 1 hour then steam distilled until no trace of product is noted condensing in the distillate. The distillate is extracted with ether, dried (magnesium sulfate) concentrated and distilled to give 7.8 g. of product, b.p. 148°-152° at 30 mm. Gas chromatography analysis shows this to be greater than 95% pure.

後処理

  1. customis kept below 5° at all times
  2. additionThis solution is then added to a stirred suspension of 18 g
  3. customat room temperature
  4. distillationsteam distilled until no trace of product
  5. customcondensing in the distillate
  6. extractionThe distillate is extracted with ether
  7. dry with materialdried (magnesium sulfate)
  8. concentrationconcentrated
  9. distillationdistilled
  10. customto give 7.8 g

出典と根拠

ORDレコード
ord-27a76dea11004c9f8398b28054f81517
出典データセット
uspto-grants-1977_06
特許番号
US04032639

反応ノート

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