Thionyl Chloride → 2-(2,5-Dichloro-phenoxy)-5-fluoro-nicotinoyl chloride

HRID 1877407노트

반응식

HRID 1877407 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:3]=1[O:4][C:5]1[N:13]=[CH:12][C:11]([F:14])=[CH:10][C:6]=1[C:7](O)=[O:8].S(Cl)([Cl:22])=O>ClCCl>[Cl:1][C:2]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:3]=1[O:4][C:5]1[N:13]=[CH:12][C:11]([F:14])=[CH:10][C:6]=1[C:7]([Cl:22])=[O:8]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 673674432-(2,5-Dichloro-phenoxy)-5-fluoro-nicotinic acid

생성물 1

HCID 866412572-(2,5-Dichloro-phenoxy)-5-fluoro-nicotinoyl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-(2,5-dichloro-phenoxy)-5-fluoro-nicotinic acid (2.14 g, 7.08 mmol, 1.0 equiv; Example 80, Step 1) in dichloromethane (15 mL) was added thionyl chloride (16.4 g, 10 mL, 138 mmol, 19.5 equiv; [CAS RN 7719-09-7]) and the reaction mixture heated to reflux for 2 h. The reaction mixture was concentrated under reduced pressure and remaining thionyl chloride removed by azotropic distillation with toluene. The crude material was used in the consecutive reaction step without further purification.

후처리

  1. temperaturethe reaction mixture heated
  2. temperatureto reflux for 2 h
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customremoved by azotropic distillation with toluene
  5. customThe crude material was used in the consecutive reaction step without further purification

출처 및 근거

ORD 기록
ord-667192e8f1cc4b27be8f2b9492723848
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309734B2

반응 노트

불러오는 중…