Dimethylformamide → 2,4-Difluoro-5-iodobenzoyl chloride

HRID 1670793

반응식

HRID 1670793 반응식
[F:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([I:12])=[CH:7][C:3]=1[C:4](O)=[O:5].S(Cl)([Cl:15])=O.CN(C=O)C>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([I:12])=[CH:7][C:3]=1[C:4]([Cl:15])=[O:5]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 111297952,4-Difluoro-5-iodobenzoic acid

생성물 1

HCID 577339872,4-Difluoro-5-iodobenzoyl chloride

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
60 °C

실험 절차

To a solution of 11 (74.0 g, 260 mmol) in toluene (370 mL) was added thionyl chloride (95 mL, 1300 mmol) in DMF (2.5 mL, 26 mmol) and the mixture was heated to reflux for 4 h. The mixture was cooled to approximately 60° C. and filtered to remove insoluble material. The filtrate was concentrated under reduced pressure and residual thionyl chloride was co-evaporated with toluene (2×120 mL) to give crude 12 which was used without purification.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 4 h
  3. filtrationfiltered
  4. customto remove insoluble material
  5. concentrationThe filtrate was concentrated under reduced pressure and residual thionyl chloride
  6. customto give crude 12 which
  7. customwas used without purification

출처 및 근거

ORD 기록
ord-c4d12b2e96734e9aa9427c510d143ef6
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994194B2

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