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

HRID 548632
ノート
印刷プレビュー

反応式

HRID 548632 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-863f414d56864102ba5e8c423b01b6ad
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943605B2

反応ノート

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