Hydrochloric Acid → 3-Ethoxyoxan-4-one

HRID 1044557ノート

反応式

HRID 1044557 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 235335993-Ethoxyoxan-4-one収率 97.7%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 21881883Oxolane--water (1/1)溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5985b3823d03404e800247705be0f455
出典データセット
uspto-grants-2013_10
特許番号
US08563582B2

反応ノート

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