Sodium Bicarbonate → 1,3-Dihydroxypropan-2-yl 4-methylbenzenesulfonate

HRID 379958노트

반응식

HRID 379958 반응식
C1([C@H]2O[C@@H:11]([O:13][S:14]([C:17]3[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=3)(=[O:16])=[O:15])[CH2:10]CO2)C=CC=CC=1.Cl.[O:25]1CCOC[CH2:26]1.C([O-])(O)=[O:32].[Na+]>CO>[C:20]1([CH3:23])[CH:19]=[CH:18][C:17]([S:14]([O:13][CH:11]([CH2:10][OH:32])[CH2:26][OH:25])(=[O:15])=[O:16])=[CH:22][CH:21]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 204431481,4-Dioxane hydrochlorideHCID 86583790cis-2-Phenyl-4-(p-toluenesulfonyloxy)-1,3-dioxane

생성물 1

HCID 103772501,3-Dihydroxypropan-2-yl 4-methylbenzenesulfonate수율 100%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 50 ml of methanol were dissolved 5.00 g of cis-2-phenyl-4-(p-toluenesulfonyloxy)-1,3-dioxane, and 5 ml of a 4N HCl-dioxane solution were added to the solution, followed by stirring of the resulting mixture at room temperature for 2 hours. To the reaction mixture were added 3.5 g of NaHCO3 powder, and the mixture was stirred for 10 minutes. Then, the reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The thus obtained oil was subjected to column chromatography using silica gel and eluted with ethyl acetate to obtain 3.70 g (yield: 100%) of the title compound as an oil.

후처리

  1. additionwere added to the solution
  2. stirringthe mixture was stirred for 10 minutes
  3. filtrationThen, the reaction mixture was filtered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. washeluted with ethyl acetate

출처 및 근거

ORD 기록
ord-df28eff20f1a42068e1189d482a2b271
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06300357B1

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