Hydrochloric Acid → 3-Ethoxyoxan-4-one

HRID 1044557노트

반응식

HRID 1044557 반응식
[CH2:1]([O:3][CH:4]1[C:9](OC)([O:10]C)[CH2:8][CH2:7][O:6][CH2:5]1)[CH3:2].Cl>C1COCC1.O.CCOC(C)=O>[CH2:1]([O:3][CH:4]1[C:9](=[O:10])[CH2:8][CH2:7][O:6][CH2:5]1)[CH3:2]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 579387433-Ethoxy-4,4-dimethoxytetrahydro-2H-pyran

생성물 1

HCID 235335993-Ethoxyoxan-4-one수율 97.7%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 21881883Oxolane--water (1/1)용매

실험 절차

To a solution of 3-ethoxy-4,4-dimethoxytetrahydro-2H-pyran (2.1 g, 11 mmol) in THF/water (50 mL/10 mL) was added concentrated HCl (6 mL). After being stirred at room temperature for 1 h, the mixture was diluted with EtOAc. The organic layer was separated and the aqueous layer was extracted with ether five times. The combined organic layers were dried over MgSO4, filtered and concentrated to give 1.55 g (97%) of the desired product 1H NMR (CDCl3) δ 4.30-3.50 (7H, m), 2.62-2.57 (2H, m), 1.30-1.20 (3H, t, J=5 Hz).

후처리

  1. customThe organic layer was separated
  2. extractionthe aqueous layer was extracted with ether five times
  3. dry with materialThe combined organic layers were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5985b3823d03404e800247705be0f455
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563582B2

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