Thionyl Chloride → 2,6-Dichloro-4-iodobenzoyl chloride

HRID 2366217ノート

反応式

HRID 2366217 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]([I:11])[CH:8]=[C:7]([Cl:12])[C:3]=1[C:4](O)=[O:5].S(Cl)([Cl:15])=O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:10]=[C:9]([I:11])[CH:8]=[C:7]([Cl:12])[C:3]=1[C:4]([Cl:15])=[O:5]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 513418772,6-Dichloro-4-iodobenzoic acid

生成物 1

HCID 866489582,6-Dichloro-4-iodobenzoyl chloride収率 99%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 2,6-dichloro-4-iodobenzoic acid (5.50 g, 17.4 mmol) in thionyl chloride (52 mL) was heated under reflux for 2 hours then diluted with toluene and concentrated under reduced pressure. The resultant residue was partitioned between EtOAc and saturated aqueous sodium bicarbonate solution. The organic layer was dried over Na2SO4 and concentrated under reduced pressure to give the desired compound as a yellow oil (5.75 g, 99% yield). 1H NMR (400 MHz, CDCl3) δ 7.75 (s, 2H).

後処理

  1. temperatureunder reflux for 2 hours
  2. concentrationconcentrated under reduced pressure
  3. customThe resultant residue was partitioned between EtOAc and saturated aqueous sodium bicarbonate solution
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-c136f3c39283497a82de3e10f43af110
出典データセット
uspto-grants-2014_04
特許番号
US08697708B2

反応ノート

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