p-Toluenesulfonic acid → Methyl beta-dihydropyranyloxyisovalerate

HRID 374393

반응식

HRID 374393 반응식
[OH:1][C:2]([CH3:9])([CH3:8])[CH2:3][C:4]([O:6][CH3:7])=[O:5].[O:10]1[CH:15]=[CH:14][CH2:13][CH2:12][CH2:11]1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(OCC)C>[O:10]1[CH:11]=[CH:12][CH2:13][CH2:14][CH:15]1[O:1][C:2]([CH3:9])([CH3:8])[CH2:3][C:4]([O:6][CH3:7])=[O:5]

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 80803,4-dihydro-2H-pyranHCID 521979Methyl 3-hydroxy-3-methylbutanoate

생성물 1

HCID 86749184Methyl beta-dihydropyranyloxyisovalerate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

In 50 ml of 7 wt. % hydrochloric acid methanol solution was dissolved 1.18 g of β-hydroxyisovaleric acid, and an reaction was allowed to proceed at room temperature overnight. The solvent was removed from the solution as reacted by distillation under a reduced pressure to obtain 1.30 g of crude methyl β-hydroxyisovalerate. The crude methyl β-hydroxyisovalerate was dissolved in diethyl ether, and 0.91 g of 3,4-dihydro-2H-pyran and a catalytic amount of p-toluenesulfonic acid were added thereto. Stirring was continued at room temperature overnight for reaction. The resultant reaction mixture was washed with a saturated aqueous solution of sodium hydrogencarbonate and then with water and dried over magnesium sulfate. The solvent was removed from the dried reaction mixture by distillation under a reduced pressure to obtain 1.98 g of crude methyl β-dihydropyranyloxyisovalerate.

후처리

  1. customwas continued at room temperature overnight for reaction
  2. customThe resultant reaction mixture
  3. washwas washed with a saturated aqueous solution of sodium hydrogencarbonate
  4. dry with materialwith water and dried over magnesium sulfate
  5. customThe solvent was removed from the dried reaction mixture by distillation under a reduced pressure

출처 및 근거

ORD 기록
ord-31b383d7b8dd4fbeba9fb7a0c3422862
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05480580

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