Potassium Carbonate → 3-Octanone

HRID 653513

반응식

HRID 653513 반응식
[OH2:1].[C:2]1([CH3:12])[CH:7]=[CH:6][C:5](S(O)(=O)=O)=[CH:4][CH:3]=1.[C:13](=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH3:13][CH2:3][C:4](=[O:1])[CH2:5][CH2:6][CH2:7][CH2:2][CH3:12]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 2467283-Octanone수율 68%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of the product obtained in Example IV (2.7 g, 0.017 mol) and p-toluenesulfonic acid monohydrate (0.023) g, 0.12 mmol) in dry toluene (200 ml) was allowed to reflux through a Soxhlet extractor for 2 hours. The Soxhlet thimble was charged with Type 4 A molecular sieves (16 g). After the solution was cooled to room temperature, anhydrous potassium carbonate (5 g, 0.036 mol) was added to the solution, and the mixture was stirred at room temperature for 30 min. The mixture was filtered and subjected to rotary evaporation to afford a slightly yellow wax at a 68% yield. Recrystallization from ethyl ether gave white crystals having a melting point of 69° C.

후처리

  1. temperatureto reflux through a Soxhlet extractor for 2 hours
  2. additionThe Soxhlet thimble was charged with Type 4 A molecular sieves (16 g)
  3. filtrationThe mixture was filtered
  4. customsubjected to rotary evaporation
  5. customto afford a slightly yellow wax at a 68% yield
  6. customRecrystallization from ethyl ether
  7. customgave white crystals

출처 및 근거

ORD 기록
ord-4fbb49309d13425a88d57267148968d2
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04677190

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