Ethyl Acetate → HCID 68784889、化合物

HRID 2383849

反応式

HRID 2383849 の反応式
Cl[CH2:2][CH2:3][CH2:4][NH:5][C:6]([NH:8][C:9]1[CH:10]=[N:11][CH:12]=[CH:13][C:14]=1[CH3:15])=[O:7].[H-].[Na+].C(OC(=O)C)C>CN(C=O)C.C1COCC1>[CH3:15][C:14]1[CH:13]=[CH:12][N:11]=[CH:10][C:9]=1[N:8]1[CH2:2][CH2:3][CH2:4][NH:5][C:6]1=[O:7]

参加物

6

反応物 3

HCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 687869921-(3-Chloro-propyl)-3-(4-methyl-pyridin-3-yl)-urea

生成物 1

HCID 68784889HCID 68784889、化合物収率 96.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

1-(3-Chloro-propyl)-3-(4-methyl-pyridin-3-yl)-urea (I-130a: 2 g, 9.25 mmol) in dry DMF (15 mL) was added to a stirred mixture of sodium hydride (330 mg, 13.87 mmol) in THF (30 mL) at 0° C. The reaction was stirred at room temperature for 1 hour. The reaction was monitored by TLC (100% ethylacetate). The reaction mixture was quenched with MeOH at 0° C., concentrated under reduced pressure and partitioned between ice water and chloroform. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated under reduced pressure to afford 1.7 g (96.5% yield) of 1-(4-methyl-pyridin-3-yl)-tetrahydro-pyrimidin-2-one.

後処理

  1. customThe reaction mixture was quenched with MeOH at 0° C.
  2. concentrationconcentrated under reduced pressure
  3. custompartitioned between ice water and chloroform
  4. washThe organic layer was washed with brine solution
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-90e862bc69a344388e22a43af32a1fd1
出典データセット
uspto-grants-2012_09
特許番号
US08263635B2

関連ノート

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