Iodoethane → 3-Ethoxy-2-methyl-4H-pyran-4-one

HRID 912653ノート

反応式

HRID 912653 の反応式
[OH:1][C:2]1[C:7](=[O:8])[CH:6]=[CH:5][O:4][C:3]=1[CH3:9].[OH-].[Na+].[CH2:12](I)[CH3:13]>CO.O>[CH2:12]([O:1][C:2]1[C:7](=[O:8])[CH:6]=[CH:5][O:4][C:3]=1[CH3:9])[CH3:13]

参加物

6

反応物 3

HCID 6340IodoethaneHCID 8369MaltolHCID 14798Sodium Hydroxide

生成物 1

HCID 98340133-Ethoxy-2-methyl-4H-pyran-4-one収率 71.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

3-Hydroxy-2-methyl-4-pyrone (10 g, 79.4 mmol) was dissolved in methanol (10 mL) and sodium hydroxide (3.49 g, 87.3 mmol) in water (8 mL) was added, followed by ethyl iodide (6.97 mL, 87.3 mmol). The reaction mixture was stirred under reflux overnight. The reaction mixture was then partitioned between water (50 mL) and CH2Cl2 (100 mL). The organic phase was washed with sodium hydroxide (5%, aq.), water, dried (MgSO4) and evaporated to give the title product (8.7 g, 71%) as a solid. The crude product was used in the next step without further purification.

後処理

  1. temperatureunder reflux overnight
  2. customThe reaction mixture was then partitioned between water (50 mL) and CH2Cl2 (100 mL)
  3. washThe organic phase was washed with sodium hydroxide (5%, aq.), water
  4. dry with materialdried (MgSO4)
  5. customevaporated

出典と根拠

ORDレコード
ord-eb17e2879cbb458f92d7c828803f90e4
出典データセット
uspto-grants-2011_09
特許番号
US08026244B2

反応ノート

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