Thionyl Chloride → 2-Methyl-6-(trifluoromethyl)nicotinoyl chloride

HRID 890137

反応式

HRID 890137 の反応式
S(Cl)([Cl:3])=O.[CH3:5][C:6]1[N:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[CH:11][C:7]=1[C:8](O)=[O:9]>C1(C)C=CC=CC=1>[CH3:5][C:6]1[C:7]([C:8]([Cl:3])=[O:9])=[CH:11][CH:12]=[C:13]([C:15]([F:18])([F:17])[F:16])[N:14]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 27756832-Methyl-6-(trifluoromethyl)nicotinic acid

生成物 1

HCID 27756752-Methyl-6-(trifluoromethyl)nicotinoyl chloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Thionyl chloride (4.35 g, 36.5 mmol) was added to a mixture of 2-methyl-6-trifluoromethyl nicotinic acid (5.00 g, 24.4 mmol) in 75 mL of toluene and the mixture was heated at reflux for 3 hours. The reaction was cooled to room temperature and the solvent was removed under reduced pressure. Excess thionyl chloride was removed by azeotrope with toluene. The resultant acid chloride was used as is in Example 4, Step B.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 3 hours
  3. customthe solvent was removed under reduced pressure
  4. customExcess thionyl chloride was removed by azeotrope with toluene

出典と根拠

ORDレコード
ord-bfc8184727d142a799132f5776391110
出典データセット
uspto-grants-2006_02
特許番号
US06995178B2

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