Hydrochloric Acid → HCID 23358997、化合物

HRID 232664ノート

反応式

HRID 232664 の反応式
S(=O)(=O)(O)O.N([O-])=O.[Na+].[F:10][C:11]1[C:17]([F:18])=[C:16]([CH3:19])[C:15]([F:20])=[CH:14][C:12]=1N.[ClH:21]>C(O)(=O)C.[Cu]Cl>[F:18][C:17]1[C:11]([F:10])=[C:12]([Cl:21])[CH:14]=[C:15]([F:20])[C:16]=1[CH3:19]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 184250192,3,5-Trifluoro-4-methylanilineHCID 23668193Sodium Nitrite

生成物 1

HCID 23358997HCID 23358997、化合物

試薬・触媒・溶媒 2

HCID 62652Cuprous chloride触媒HCID 176Acetic Acid溶媒

反応条件

温度
70 °C

実験手順

To conc. sulfuric acid (3 ml) is added sodium nitrite (0.3 g). The mixture is stirred at 70° C. for 10 minutes and then cooled to below 40° C. and thereto a solution of 2,3,5-trifluoro-4-methylaniline (0.48 g) in acetic acid (5 ml) is added dropwise below 40° C. After stirring for 30 minutes, the reaction mixture is added dropwise to a solution of copper (I) chloride (1.04 g) in conc. hydrochloric acid (10.4 ml) and the mixture is stirred at 80° C. for 30 minutes and then cooled. The resultant mixture is poured into ice-water, extracted with dichloromethane, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and purified by silica-gel column-chromatography (eluent; dichloromethane: n-hexane=1:4) to give 2,3,6-trifluoro-4-chlorotoluene (0.22 g).

後処理

  1. temperaturecooled to below 40° C.
  2. stirringAfter stirring for 30 minutes
  3. stirringthe mixture is stirred at 80° C. for 30 minutes
  4. temperaturecooled
  5. extractionextracted with dichloromethane
  6. washthe extract is washed with water
  7. customdried
  8. distillationThe solvent is distilled off under reduced pressure
  9. custompurified by silica-gel column-chromatography (eluent; dichloromethane: n-hexane=1:4)

出典と根拠

ORDレコード
ord-9eea9288c44845239e59941f5d1a9cf0
出典データセット
uspto-grants-1997_01
特許番号
US05591744

反応ノート

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