Sodium hydride → 1-(4-Methylpyridin-3-yl)imidazolidin-2-one

HRID 80038

반응식

HRID 80038 반응식
Cl[CH2:2][CH2:3][NH:4][C:5]([NH:7][C:8]1[CH:9]=[N:10][CH:11]=[CH:12][C:13]=1[CH3:14])=[O:6].[H-].[Na+]>CN(C=O)C.C1COCC1>[CH3:14][C:13]1[CH:12]=[CH:11][N:10]=[CH:9][C:8]=1[N:7]1[CH2:2][CH2:3][NH:4][C:5]1=[O:6]

참가 물질

5

반응물 2

HCID 24758Sodium hydrideHCID 148343251-(2-Chloro-ethyl)-3-(4-methyl-pyridin-3-yl)-urea

생성물 1

HCID 596361701-(4-Methylpyridin-3-yl)imidazolidin-2-one수율 91.8%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

1-(2-Chloro-ethyl)-3-(4-methyl-pyridin-3-yl)-urea (I-14a: 8.5 g, 39.96 mmol) in dry DMF (150 mL) was added to a stirred mixture of sodium hydride (2.87 g, 59.94 mmol) in THF (150 mL) at 0° C. The reaction temperature was maintained at room temperature for 30 minutes. The reaction was monitored by TLC. 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 dried over Na2SO4, and concentrated under reduced pressure to afford 6.5 g (91% yield) of 1-(4-methyl-pyridin-3-yl)-imidazolidin-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. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e121337205f84b488c01f8c056573960
출처 데이터셋
uspto-grants-2014_09
특허 번호
USRE045173E1

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