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Potassium Carbonate → 4-(Pyrrolidin-1-ylmethyl)-1,3-oxazolidin-2-one

HRID 548632
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반응식

HRID 548632 반응식
C(=O)([O-])[O-].[K+].[K+].[NH:7]1[CH2:11][CH2:10][CH2:9][CH2:8]1.CC1C=CC(S(O[CH2:23][CH:24]2[CH2:28][O:27][C:26](=[O:29])[NH:25]2)(=O)=O)=CC=1>C(#N)C>[N:7]1([CH2:23][CH:24]2[CH2:28][O:27][C:26](=[O:29])[NH:25]2)[CH2:11][CH2:10][CH2:9][CH2:8]1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 31268PyrrolidineHCID 14456891(2-Oxo-1,3-oxazolidin-4-yl)methyl 4-methylbenzene-1-sulfonate

생성물 1

HCID 575502564-(Pyrrolidin-1-ylmethyl)-1,3-oxazolidin-2-one수율 92%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Potassium carbonate (0.62 g, 4.5 mmol, 2 eq) and pyrrolidine (0.28 ml, 3.37 mmol, 1.5 eq) are added to a solution of (2-oxo-1,3-oxazolidin-4-yl)methyl 4-methylbenzenesulfonate a91 (0.62 g, 2.25 mmol, 1 eq) in acetonitrile (22 ml). The mixture is heated at reflux overnight. After cooling, the mixture is filtered and the solid is washed with acetonitrile. The acetonitrile phases are concentrated in vacuo. The residue is taken up in dichloromethane, heated, filtered and washed with dichloromethane. The dichloromethane phases are concentrated in vacuo to give 0.35 g of 4-(pyrrolidin-1-ylmethyl)-1,3-oxazolidin-2-one a92 as a yellow oil.

후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux overnight
  3. temperatureAfter cooling
  4. filtrationthe mixture is filtered
  5. washthe solid is washed with acetonitrile
  6. concentrationThe acetonitrile phases are concentrated in vacuo
  7. temperatureheated
  8. filtrationfiltered
  9. washwashed with dichloromethane
  10. concentrationThe dichloromethane phases are concentrated in vacuo

출처 및 근거

ORD 기록
ord-863f414d56864102ba5e8c423b01b6ad
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07943605B2

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