Hydrochloric Acid → 2-((3-Fluorophenyl)amino)-4-(propylamino)pyrimidine-5-carboxylic acid

HRID 2284708노트

반응식

HRID 2284708 반응식
[F:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[N:14]=[C:13]([NH:15][CH2:16][CH2:17][CH3:18])[C:12]([C:19]([O:21]CC)=[O:20])=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1.Cl>C(O)C.O1CCCC1.[OH-].[Na+]>[F:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[N:14]=[C:13]([NH:15][CH2:16][CH2:17][CH3:18])[C:12]([C:19]([OH:21])=[O:20])=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 90052261HCID 90052261, 화합물

생성물 1

HCID 900521172-((3-Fluorophenyl)amino)-4-(propylamino)pyrimidine-5-carboxylic acid수율 57.7%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매HCID 14798Sodium Hydroxide용매2회

반응 조건

온도
50 °C

실험 절차

To a solution of ethyl 2-((3-fluorophenyl)amino)-4-(propylamino)pyrimidine-5-carboxylate (E3, 247 mg) in ethanol (3 mL) and tetrahydrofuran (1.5 mL), 2.0 mol/L aqueous sodium hydroxide (0.78 mL) was added at room temperature, and the mixture was stirred at 50° C. for 1 hour. To the reaction mixture, 2.0 mol/L aqueous sodium hydroxide (0.39 mL) was added at 50° C., and the mixture was stirred at the same temperature for 3 hours. The reaction mixture was cooled to room temperature, and then 1.0 mol/L aqueous hydrochloric acid was added to the reaction mixture until the mixture became acidic. The solid matter was taken by filtration, washed with water, and then dried under reduced pressure to obtain 2-((3-fluorophenyl)amino)-4-(propylamino)pyrimidine-5-carboxylic acid (E22, 130 mg).

후처리

  1. stirringthe mixture was stirred at the same temperature for 3 hours
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationThe solid matter was taken by filtration
  4. washwashed with water
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-dd507d80924b4c28b97841d28f0ca52f
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09145415B2

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