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

HRID 1877407ノート

反応式

HRID 1877407 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-667192e8f1cc4b27be8f2b9492723848
出典データセット
uspto-grants-2012_11
特許番号
US08309734B2

反応ノート

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