Ethyl Acetate → HCID 68784889, 화합물

HRID 2383849

반응식

HRID 2383849 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

HCID 68784889HCID 68784889, 화합물수율 96.5%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-90e862bc69a344388e22a43af32a1fd1
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08263635B2

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