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

HRID 875061

반응식

HRID 875061 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 111297952,4-Difluoro-5-iodobenzoic acid수율 99.6%

시약·촉매·용매 1

HCID 62406Trifluoromethanesulfonic acid용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7ba54a8e6b084dc0ba2d8f5b498bb7b7
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08981103B2

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