Hydrochloric Acid → 3-Ethoxyoxan-4-one

HRID 1436757노트

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HRID 1436757 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-d00e169bc8974358813251856888fdb3
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618970B2

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