Acetone → HCID 60091526, 화합물

HRID 353221노트

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HRID 353221 반응식
[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]

참가 물질

6

반응물 4

HCID 180AcetoneHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 20735499HCID 20735499, 화합물

생성물 1

HCID 60091526HCID 60091526, 화합물수율 81%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-b7b3d27b5f964b0ab3a1c0fad4f83037
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06750232B2

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