Water → 2,4-Difluoro-5-iodobenzoic acid

HRID 875061

反応式

HRID 875061 の反応式
[F:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[I:12]N1C(=O)CCC1=O.O>FC(F)(F)S(O)(=O)=O>[F:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([I:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

5

反応物 3

HCID 962WaterHCID 741022,4-Difluorobenzoic acidHCID 120273N-Iodosuccinimide

生成物 1

HCID 111297952,4-Difluoro-5-iodobenzoic acid収率 99.6%

試薬・触媒・溶媒 1

HCID 62406Trifluoromethanesulfonic acid溶媒

反応条件

温度
50 °C

実験手順

2,4-Difluorobenzoic acid (100 g, 633 mmol) was dissolved in trifluoromethanesulfonic acid (400 ml) and N-iodosuccinimide (157 g, 696 mmol) was added by portions at not more than 5° C. After the completion of the addition, the mixture was stirred at 50° C. for 1.5 hr. The reaction mixture was poured into iced water, and the mixture was stirred for 1 hr. The precipitated solid was collected by filtration, washed successively with water and hexane, and vacuum dried to give 2,4-difluoro-5-iodobenzoic acid (179 g yield quantitative) as a white solid.

後処理

  1. additionAfter the completion of the addition
  2. stirringthe mixture was stirred for 1 hr
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed successively with water and hexane, and vacuum
  5. customdried

出典と根拠

ORDレコード
ord-7ba54a8e6b084dc0ba2d8f5b498bb7b7
出典データセット
uspto-grants-2015_03
特許番号
US08981103B2

関連ノート

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