Hydrochloric Acid → {4-[2-(2-Methoxy-phenyl)-ethyl]-pyridin-2-yl}-urea

HRID 1023450노트

반응식

HRID 1023450 반응식
C(=O)([O-])[O-].[K+].[K+].C([NH:15][C:16]([NH:18][C:19]1[CH:24]=[C:23]([CH2:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[O:33][CH3:34])[CH:22]=[CH:21][N:20]=1)=[O:17])(=O)C1C=CC=CC=1.Cl>C(O)C>[CH3:34][O:33][C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=1[CH2:26][CH2:25][C:23]1[CH:22]=[CH:21][N:20]=[C:19]([NH:18][C:16]([NH2:15])=[O:17])[CH:24]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 690823961-Benzoyl-3-{4-[2-(2-methoxy-phenyl)-ethyl]-pyridin-2-yl}-urea

생성물 1

HCID 69082641{4-[2-(2-Methoxy-phenyl)-ethyl]-pyridin-2-yl}-urea

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
85 °C

실험 절차

Potassium carbonate (93.2 mg, 0.674 mmol) is added to a solution of the crude 1-benzoyl-3-{4-[2-(2-methoxy-phenyl)-ethyl]-pyridin-2-yl}-urea (211 mg) in absolute ethanol (3 mL), and the mixture is heated at 85° C. After 2 hours, the mixture is cooled to room temperature, neutralized with 1 M aqueous HCl to pH 7-8, and stirred over night. The mixture is filtered, and the solids are washed with EtOH (2×0.5 mL) and air dried. The solids are partitioned between ethyl acetate (10 mL) and saturated aqueous NaHCO3 (3 mL). The organic layer is dried over MgSO4, filtered and concentrated to give the titled product.

후처리

  1. temperaturethe mixture is cooled to room temperature
  2. filtrationThe mixture is filtered
  3. washthe solids are washed with EtOH (2×0.5 mL) and air
  4. customdried
  5. customThe solids are partitioned between ethyl acetate (10 mL) and saturated aqueous NaHCO3 (3 mL)
  6. dry with materialThe organic layer is dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f2546606d5c84d1f83bd843961a0a03f
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722709B2

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