Potassium Hydroxide → 2-(3-Chlorophenylamino)-4-trifluoromethylpyrimidine-5-carboxylic acid

HRID 1868369ノート

反応式

HRID 1868369 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[N:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[C:12]([C:19]([O:21]CC3C=CC=CC=3)=[O:20])=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1.[OH-].[K+]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[N:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[C:12]([C:19]([OH:21])=[O:20])=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 16719547Benzyl 2-(3-chlorophenylamino)-4-trifluoromethylpyrimidine-5-carboxylate

生成物 1

HCID 167196552-(3-Chlorophenylamino)-4-trifluoromethylpyrimidine-5-carboxylic acid収率 94%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of benzyl 2-(3-chlorophenylamino)-4-trifluoromethyl-pyrimidine-5-carboxylate (0.50 g) in ethanol (15 ml) was added a solution of potassium hydroxide (205 mg) in ethanol (10 ml) and the solution stirred at reflux for 15 h. Ethanol was removed under reduced pressure and water (15 ml) added. The solution was washed with ether and concentrated hydrochloric acid 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-(3-chlorophenylamino)-4-trifluoromethylpyrimidine-5-carboxylic acid (366 mg).

後処理

  1. temperatureat reflux for 15 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. additionadded
  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-0a8863d90b884e32be04b4aec80d7761
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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