Oxalyl chloride → 2-Methoxy-4,6-bis(trifluoromethyl)benzoyl chloride

HRID 20835

反応式

HRID 20835 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:9]=[C:8]([C:16]([F:19])([F:18])[F:17])[C:4]=1[C:5](O)=[O:6].C(Cl)(=O)C([Cl:23])=O>C(Cl)Cl.CN(C=O)C>[CH3:1][O:2][C:3]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:9]=[C:8]([C:16]([F:19])([F:18])[F:17])[C:4]=1[C:5]([Cl:23])=[O:6]

参加物

5

反応物 2

HCID 65578Oxalyl chlorideHCID 27412872-Methoxy-4,6-bis(trifluoromethyl)benzoic acid

生成物 1

HCID 179993452-Methoxy-4,6-bis(trifluoromethyl)benzoyl chloride収率 109.3%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(methyloxy)-4,6-bis(trifluoromethyl)benzoic acid (20.2 g; 70.14 mmol) in dry DCM (400 mL), at 0° C., was added dropwise oxalyl chloride (13.4 mL; 154.31 mmol) followed by dry DMF (5 drops). The reaction was allowed to reach room temperature. After overnight stirring the solvent was evaporated in vacuo to get the title product (23.5 g) as a yellow slurry used without further purification.

後処理

  1. customto reach room temperature
  2. customwas evaporated in vacuo

出典と根拠

ORDレコード
ord-865399f9efde4960829c7c9e0ae9bec4
出典データセット
uspto-grants-2010_06
特許番号
US07745642B2

関連ノート

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