Hydrochloric Acid → 1,2,3-Trichloro-5-(trifluoromethyl)benzene

HRID 851348ノート

反応式

HRID 851348 の反応式
[Cl:1][C:2]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[C:5]([Cl:13])[C:3]=1N.N([O-])=O.[Na+].[ClH:18]>O>[Cl:1][C:2]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[C:5]([Cl:13])[C:3]=1[Cl:18]

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 1410944-Amino-3,5-dichlorobenzotrifluorideHCID 23668193Sodium Nitrite

生成物 1

HCID 27333991,2,3-Trichloro-5-(trifluoromethyl)benzene

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-6 °C

実験手順

2,6-Dichloro-4-trifluoromethylaniline (3.3 kg) in concentrated hydrochloric acid (25 liters) was stirred for 1 hour and then cooled to -6° C. A solution of sodium nitrite (1.41 kg) in water (3 liters) was added over a period of 4 hours keeping the temperature between -5° and -12°. The mixture was then stirred between -5° and 0° until all solid had dissolved (3.5 hours). The mixture was then added in 2 liter portions over a period of 35 minutes to a solution of cuprous chloride (1.5 kg) in concentrated hydrochloric acid with stirring. The dark solution was left to stand for 30 minutes, filtered, and extracted with dichloromethane (1×15 liters, then 2×10 liters). The extracts were washed with water (2×25 liters) dried (MgSO4) and evaporated under reduced pressure to give 3,4,5-trichlorobenzotrifluoride (2.2 kg) with a boiling range of 98°- 100°/40 Torr.

後処理

  1. customthe temperature between -5° and -12°
  2. dissolutionhad dissolved (3.5 hours)
  3. stirringwith stirring
  4. waitThe dark solution was left
  5. filtrationfiltered
  6. extractionextracted with dichloromethane (1×15 liters
  7. washThe extracts were washed with water (2×25 liters)
  8. dry with materialdried (MgSO4)
  9. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-3c45717266f34d9888652d52085fbb56
出典データセット
uspto-grants-1983_05
特許番号
US04384135

反応ノート

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