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

HRID 1023450ノート

反応式

HRID 1023450 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
85 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f2546606d5c84d1f83bd843961a0a03f
出典データセット
uspto-grants-2014_05
特許番号
US08722709B2

反応ノート

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