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

HRID 1670793ノート

反応式

HRID 1670793 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 577339872,4-Difluoro-5-iodobenzoyl chloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c4d12b2e96734e9aa9427c510d143ef6
出典データセット
uspto-grants-2011_08
特許番号
US07994194B2

反応ノート

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