Potassium Carbonate → 3-(3-Oxo-butoxy)-chromen-2-one

HRID 592126

反応式

HRID 592126 の反応式
[OH:1][C:2]1[C:3](=[O:12])[O:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.C(=O)([O-])[O-].[K+].[K+].C1OCCOCCOCCOCCOCCOC1.Cl[CH2:38][CH2:39][C:40](=[O:42])[CH3:41]>C1COCC1>[O:42]=[C:40]([CH3:41])[CH2:39][CH2:38][O:1][C:2]1[C:3](=[O:12])[O:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 136503-HydroxycoumarinHCID 2855718-Crown-6HCID 806084-Chloro-2-butanone

生成物 1

HCID 867104563-(3-Oxo-butoxy)-chromen-2-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3-Hydroxy-chromen-2-one (16.2 g, 100 mmol) is dissolved into 100 mL of anhydrous THF in a three neck flask equipped with a condenser, stir bar, and argon inlet. To the mixture is added 27.6 g (200 mmol) of anhydrous potassium carbonate and 2.0 g of 18-crown-6. 4-Chloro-2-butanone (15.9 g, 150 mmol) is added and the system is refluxed for 16 hours, cooled to room temperature, filtered, and the organic solvents are removed by rotary evaporation. The solid organic residue is purified by column chromatography using 3:1 ethyl acetate:hexanes to yield 3-(3-oxo-butoxy)-chromen-2-one.

後処理

  1. customequipped with a condenser
  2. temperaturethe system is refluxed for 16 hours
  3. filtrationfiltered
  4. customthe organic solvents are removed by rotary evaporation
  5. customThe solid organic residue is purified by column chromatography

出典と根拠

ORDレコード
ord-c7c5525a42064e41aa5025e479a30888
出典データセット
uspto-grants-2016_01
特許番号
US09238712B2

関連ノート

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