Iodine → 2-Chloro-3,5-difluoro-4-methylbenzoyl chloride

HRID 34589ノート

反応式

HRID 34589 の反応式
[Cl:1]Cl.[F:3][C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([F:14])[C:12]=1[CH3:13])[C:7]([Cl:9])=[O:8].II>>[F:3][C:4]1[CH:5]=[C:6]([C:10]([Cl:1])=[C:11]([F:14])[C:12]=1[CH3:13])[C:7]([Cl:9])=[O:8]

参加物

4

反応物 3

HCID 807IodineHCID 24526ChlorineHCID 136574553,5-Difluoro-4-methylbenzoyl chloride

生成物 1

HCID 136574602-Chloro-3,5-difluoro-4-methylbenzoyl chloride収率 53.2%

実験手順

30 g of chlorine are passed into 70 g of 3,5-difluoro-4-methyl-benzoyl chloride and a spatula-tip of FeS and I2 at 40°-45°, with slight cooling. The mixture is then flushed with nitrogen, the residue is coarsely distilled and the distillate is fractionated. 44 g of 3,5-difluoro-4-methyl-6-chlorobenzoyl chloride of boiling point: 109°/16 mbar, nD20 : 1.5342 are obtained. 3,5-Difluoro-2,6-dichloro-4-methyl-benzoyl chloride of boiling point b.p: 109°/13 mbar, nD20 : 1.5274 are obtained from the last runnings.

後処理

  1. customat 40°-45°
  2. customThe mixture is then flushed with nitrogen
  3. distillationthe residue is coarsely distilled

出典と根拠

ORDレコード
ord-871f95620d28494d83205aa04269860f
出典データセット
uspto-grants-1988_08
特許番号
US04762844

反応ノート

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