Ethyl Acetate → HCID 68784889、化合物

HRID 80165

反応式

HRID 80165 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-e45793faf1d549239343b24af20e05f5
出典データセット
uspto-grants-2014_09
特許番号
USRE045173E1

関連ノート

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