Potassium Hydroxide → 2-(2,4-Dichlorophenylamino)-4-trifluoromethylpyrimidine-5-carboxylic acid

HRID 1868372ノート

反応式

HRID 1868372 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[C:13]([C:20]([O:22]C)=[O:21])=[CH:12][N:11]=1.[OH-].[K+]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:15]=[C:14]([C:16]([F:17])([F:18])[F:19])[C:13]([C:20]([OH:22])=[O:21])=[CH:12][N:11]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 167195495-Pyrimidinecarboxylic acid, 2-[(2,4-dichlorophenyl)amino]-4-(trifluoromethyl)-, methyl ester

生成物 1

HCID 167197432-(2,4-Dichlorophenylamino)-4-trifluoromethylpyrimidine-5-carboxylic acid収率 76.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of methyl 2-(2,4-dichlorophenylamino)-4-trifluoromethyl-pyrimidine-5-carboxylate (0.358 g) in ethanol (8 ml) was added a solution of potassium hydroxide (190 mg) in ethanol (8 ml) and the solution stirred at reflux for 24 h. Ethanol was removed under reduced pressure and water (15 ml) added. The solution was washed with ether and concentrated hydrochloric acid was added to adjust the acidity to pH 1. The precipitated solid was filtered, washed with water and dried in vacuo at 50° C. to afford 2-(2,4-dichlorophenylamino)-4-trifluoromethyl-pyrimidine-5-carboxylic acid (262 mg).

後処理

  1. temperatureat reflux for 24 h
  2. customEthanol was removed under reduced pressure and water (15 ml)
  3. additionadded
  4. washThe solution was washed with ether and concentrated hydrochloric acid
  5. additionwas added
  6. filtrationThe precipitated solid was filtered
  7. washwashed with water
  8. customdried in vacuo at 50° C.

出典と根拠

ORDレコード
ord-db082d1f16164efaac4b6c0a94fb0c10
出典データセット
uspto-grants-2009_12
特許番号
US07635701B2

反応ノート

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