Hydrogen Peroxide → 2,4-Dichloro-5-fluorobenzoic acid

HRID 374607

反応式

HRID 374607 の反応式
[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[C:13]([F:17])=[CH:12][C:3]=1[C:4](C1C=CC=CC=1)=[O:5].[OH:18]O>S(=O)(=O)(O)O.O>[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[C:13]([F:17])=[CH:12][C:3]=1[C:4]([OH:5])=[O:18]

参加物

5

反応物 2

HCID 784Hydrogen Peroxide2 回HCID 18997589HCID 18997589、化合物

生成物 1

HCID 6881382,4-Dichloro-5-fluorobenzoic acid収率 85.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒

実験手順

26.8 g (0.1 mol) of 2,4-dichloro-5-fluorobenzophenone are dissolved in 250 g of 96% sulfuric acid, and 17 g of 30% hydrogen peroxide solution are added at 0° C., with thorough mixing, in such a way that the temperature does not exceed 40° C. When the metered addition is complete, the temperature is allowed to drop to 20° C. and the mixture is stirred for 5 h at this temperature. If the conversion is incomplete, a further 5 g of hydrogen peroxide solution are metered in (T<40° C.) and the mixture is diluted with 1000 g of water after a further 3 h of reaction time and is subsequently stirred for 2 h. The 2,4-dichloro-5-fluorobenzoic acid which has precipitated out is filtered off and purified by recrystallization (water) to give 17.8 g (0.0852 mol, 85%) of 2,4-dichloro-5-fluorobenzoic acid melting at 144°-146° C.

後処理

  1. customdoes not exceed 40° C
  2. additionWhen the metered addition
  3. customto drop to 20° C.
  4. customare metered in (T<40° C.)
  5. stirringis subsequently stirred for 2 h
  6. customThe 2,4-dichloro-5-fluorobenzoic acid which has precipitated out
  7. filtrationis filtered off
  8. custompurified by recrystallization (water)

出典と根拠

ORDレコード
ord-f646ca80c5e9470686d0709ce74955f2
出典データセット
uspto-grants-1996_01
特許番号
US05481032

関連ノート

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