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

HRID 2366217

반응식

HRID 2366217 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 866489582,6-Dichloro-4-iodobenzoyl chloride수율 99%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c136f3c39283497a82de3e10f43af110
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697708B2

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