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

HRID 1868369

반응식

HRID 1868369 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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).

후처리

  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.

출처 및 근거

ORD 기록
ord-0a8863d90b884e32be04b4aec80d7761
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07635701B2

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