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p-Toluenesulfonic acid → HCID 54124038, 화합물

HRID 1395078
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HRID 1395078 반응식
[C:1]1(C)[CH:6]=CC(S(O)(=O)=O)=C[CH:2]=1.[OH:12][C@:13]([CH3:21])([CH2:19][OH:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15]>>[CH3:2][C:1]1([CH3:6])[O:12][C@@:13]([CH3:21])([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:19][O:20]1
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참가 물질

3

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 53737198Ethyl (2R)-2,3-dihydroxy-2-methylpropanoate

생성물 1

HCID 54124038HCID 54124038, 화합물수율 2,049.4%

실험 절차

500 mg of p-toluenesulfonic acid were added to 10.7 g of ethyl (R)-2,3-dihydroxy-2-methylpropionate, dissolved in 35 ml of dry, freshly distilled 2,2-dimethoxypropane, and the mixture was stirred at room temperature overnight. The excess dimethoxypropane was removed at 45°/12 mmHg and the residue was vigorously stirred for 30 minutes with 5 ml of 1-N sodium bicarbonate. Then, 150 ml of ether were added thereto and the aqueous phase was separated. The ether solution was washed with saturated brine and then dried over sodium sulfate. After evaporation of the solvent, the product was distilled and there were obtained 11.2 g of ethyl (R)-2,2,4-trimethyl-1,3-dioxolan-4-carboxylate in the form of a colorless liquid; boiling point 81°/15 mmHg.

후처리

  1. dissolutiondissolved in 35 ml
  • customof dry
  • customThe excess dimethoxypropane was removed at 45°/12 mmHg
  • stirringthe residue was vigorously stirred for 30 minutes with 5 ml of 1-N sodium bicarbonate
  • additionThen, 150 ml of ether were added
  • customthe aqueous phase was separated
  • washThe ether solution was washed with saturated brine
  • dry with materialdried over sodium sulfate
  • customAfter evaporation of the solvent
  • distillationthe product was distilled
  • 출처 및 근거

    ORD 기록
    ord-558deb09c654484eaf3697474d710f49
    출처 데이터셋
    uspto-grants-1980_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04201879

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