Sodium Sulfite → 2,3-Difluoro-5-iodobenzoic acid

HRID 347884

反応式

HRID 347884 の反応式
[F:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[I:12]N1C(=O)CCC1=O.S([O-])([O-])=O.[Na+].[Na+]>FC(F)(F)S(O)(=O)=O>[F:1][C:2]1[C:10]([F:11])=[CH:9][C:8]([I:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

5

反応物 3

HCID 24437Sodium SulfiteHCID 120273N-IodosuccinimideHCID 3705902,3-Difluorobenzoic acid

生成物 1

HCID 108913672,3-Difluoro-5-iodobenzoic acid収率 84%

試薬・触媒・溶媒 1

HCID 62406Trifluoromethanesulfonic acid溶媒

実験手順

2,3-Difluorobenzoic acid (5.0 g, 31.6 mmol) was dissolved in trifluoromethanesulfonic acid (25 ml), and N-iodosuccinimide (8.55 g, 38.0 mmol) was added by portions at 0° C. under an argon stream. The mixture was stirred at room temperature for 3 hrs., and the reaction solution was poured into sodium sulfite in ice water. The mixture was stirred and the precipitate was collected by filtration, washed with water and vacuum-dried to give an object product (7.5 g, yield 84%) as a pale-pink solid.

後処理

  1. stirringThe mixture was stirred
  2. filtrationthe precipitate was collected by filtration
  3. washwashed with water
  4. customvacuum-dried

出典と根拠

ORDレコード
ord-54a82cb98b75439881439e746f54f000
出典データセット
uspto-grants-2007_02
特許番号
US07176220B2

関連ノート

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