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

HRID 1868372노트

반응식

HRID 1868372 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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).

후처리

  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.

출처 및 근거

ORD 기록
ord-db082d1f16164efaac4b6c0a94fb0c10
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07635701B2

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