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Potassium Carbonate → 3-[4-(3-Hydroxybutoxy)phenyl]-5-methoxymethyl-2-oxazolidinone

HRID 1087604
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HRID 1087604 반응식
S(O[CH2:12][CH2:13][CH:14]([OH:16])[CH3:15])(C1C=CC(C)=CC=1)(=O)=O.C([O-])([O-])=O.[K+].[K+].[OH:23][C:24]1[CH:29]=[CH:28][C:27]([N:30]2[CH2:34][CH:33]([CH2:35][O:36][CH3:37])[O:32][C:31]2=[O:38])=[CH:26][CH:25]=1>CC(CC)=O>[OH:16][CH:14]([CH3:15])[CH2:13][CH2:12][O:23][C:24]1[CH:25]=[CH:26][C:27]([N:30]2[CH2:34][CH:33]([CH2:35][O:36][CH3:37])[O:32][C:31]2=[O:38])=[CH:28][CH:29]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 131054003-(4-Hydroxyphenyl) 5-methoxymethyl 2-oxazolidinoneHCID 132043233-Hydroxybutyl 4-methylbenzenesulfonate

생성물 1

HCID 97961793-[4-(3-Hydroxybutoxy)phenyl]-5-methoxymethyl-2-oxazolidinone수율 70%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

To a solution of 27.5 g (0.112 mol) of 1-tosyloxy-3-butanol in 250 ml of methylethylketone, are added 28.2 g (0.2 mol) of K2CO3 and 22.8 g (0.102 mol) of 3-(4-hydroxyphenyl)-5-methoxymethyl-2-oxazolidinone (code number MD 780232). The mixture is heated under reflux for 4 h 30. After filtration and concentration, the residue is taken up in 200 ml of CH2Cl2, the organic phase is washed with NaCl saturated water, dried over Na2SO4 and concentrated. After purification by flash chromatography silica, eluent: CH2Cl2 : 98; CH3OH: 2), the aimed product is obtained with a 70% yield, m.p.: 58° C.;

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 4 h 30
  3. filtrationAfter filtration and concentration
  4. washthe organic phase is washed with NaCl saturated water
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customAfter purification by flash chromatography silica, eluent

출처 및 근거

ORD 기록
ord-e40425e309f24b919e508ae1aa058879
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05036091

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