Acetone → HCID 60091526、化合物

HRID 353221ノート

反応式

HRID 353221 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6](=[O:14])[CH2:7][C:8](=[S:13])[O:9][CH:10]([CH3:12])[CH3:11].[C:15](=O)([O-])[O-].[K+].[K+].CC(C)=O.CI>C(OCC)(=O)C>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6](=[O:14])/[CH:7]=[C:8](/[O:9][CH:10]([CH3:11])[CH3:12])\[S:13][CH3:15]

参加物

6

反応物 4

HCID 180AcetoneHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 20735499HCID 20735499、化合物

生成物 1

HCID 60091526HCID 60091526、化合物収率 81%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

A mixture of isopropyl 3-(2-furyl)-3-oxopropanethioate (3.7 g, 17.5 mmol), potassium carbonate (7.3 g, 52.4 mmol) and acetone (15 mL) was heated under reflux for 1 hour. After cooling the mixture to 0° C., methyl iodide (2.17 mL, 34.9 mmol) was added thereto, followed by stirring at room temperature for 2 hours. After diluting the reaction solution with ethyl acetate, the insoluble matters were filtered off. The filtrate was concentrated, and then the residue was purified by silica gel column chromatography (elution solvent; ethyl acetate/hexane=1:1), to give the title compound (3.2 g, 81%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour
  3. filtrationthe insoluble matters were filtered off
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by silica gel column chromatography (elution solvent; ethyl acetate/hexane=1:1)

出典と根拠

ORDレコード
ord-b7b3d27b5f964b0ab3a1c0fad4f83037
出典データセット
uspto-grants-2004_06
特許番号
US06750232B2

反応ノート

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