Dimethylformamide → HCID 19773828、化合物

HRID 1614417ノート

反応式

HRID 1614417 の反応式
S(Cl)(Cl)=O.[F:5][C:6]1[C:14]([F:15])=[CH:13][C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][C:7]=1[C:8](O)=[O:9].C[N:21](C)C=O>>[F:5][C:6]1[C:14]([F:15])=[CH:13][C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][C:7]=1[C:8]([NH2:21])=[O:9]

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 19773825HCID 19773825、化合物

生成物 1

HCID 19773828HCID 19773828、化合物収率 86%

反応条件

温度
75 °C

実験手順

Thionyl chloride, 6.0 g (50 mmol) was added to a solution of 3.50 g (15 mmol) 2,3-difluoro-5-(trifluoromethyl) benzoic acid in 10 mL dimethylformamide. The reaction mixture was heated to 75° C. for 2 hours, cooled to room temperature and carefully added to 25 mL of ice cold ammonium hydroxide. The mixture was cooled to 0° C. and the solid product filtered, washed with water and dried to yield 3.00 g (86%) of 2,3-difluoro-5-(trifluoromethyl)benzamide m.p. 128°-130° C.

後処理

  1. temperaturecooled to room temperature
  2. temperatureThe mixture was cooled to 0° C.
  3. filtrationthe solid product filtered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-eb2648e69a7e46b9a24f2f34a8d95a9f
出典データセット
uspto-grants-1993_03
特許番号
US05196593

反応ノート

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