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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Iodine → Benzoyl chloride, 2,3-dichloro-4,5-difluoro-

HRID 2259451
ノート
印刷プレビュー

反応式

HRID 2259451 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([Cl:6])=[O:5].[Cl:13]S(O)(=O)=O.II.S(Cl)(Cl)=O>O>[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([Cl:6])=[O:5].[Cl:1][C:2]1[C:10]([Cl:13])=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([Cl:6])=[O:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 807IodineHCID 24386Thionyl ChlorideHCID 24638Chlorosulfonic acidHCID 101982172-Chloro-4,5-difluorobenzoyl chloride

生成物 2

HCID 101982172-Chloro-4,5-difluorobenzoyl chloride収率 22%HCID 10999320Benzoyl chloride, 2,3-dichloro-4,5-difluoro-収率 71%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

211 g (1 mol) of 2-chloro-4,5-difluorobenzoyl chloride are introduced into 500 g of chlorosulfonic acid, and 3 g of iodine are added. The mixture is chlorinated (10 l/h) for 1.7 h at 40° C. and then diluted with water (500 g), with stirring, the temperature being allowed to rise to 80° C. In this procedure, the acid chlorides initially present in the solvent are hydrolyzed in 2 h to the carboxylic acids, which are isolated by filtration after cooling to 0° C. After drying, the mixture is reacted with thionyl chloride (2 mol) at 80° C. and excess thionyl chloride is then distilled off. The mixture is then distilled, as indicated in Example 1, to give 46.4 g (0.22 mol, 22%) of 2-chloro-4,5-difluorobenzoyl chloride and 174.9 g (0.71 mol, 71%) of 2,3-dichloro-4,5-difluorobenzoyl chloride.

後処理

  1. additionare added
  2. customfor 1.7 h
  3. customat 40° C.
  4. customto rise to 80° C
  5. customare isolated by filtration
  6. customAfter drying
  7. distillationexcess thionyl chloride is then distilled off
  8. distillationThe mixture is then distilled

出典と根拠

ORDレコード
ord-a6e320b5fd6e4311a824435fe9c45d75
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05473095

反応ノート

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