Sulfuric Acid → 2-Methyl-2-pinanylperoxy-4-pentanone

HRID 1577960

반응식

HRID 1577960 반응식
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[C:8]12([O:18][OH:19])[CH2:16][CH:12]([C:13]1([CH3:15])[CH3:14])[CH2:11][CH2:10][CH:9]2[CH3:17].S(=O)(=O)(O)O>>[CH3:6][C:5]([O:19][O:18][C:8]12[CH2:16][CH:12]([C:13]1([CH3:14])[CH3:15])[CH2:11][CH2:10][CH:9]2[CH3:17])([CH2:4][C:2](=[O:1])[CH3:3])[CH3:7]

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 8858Mesityl oxideHCID 147175701-Pinanyl hydroperoxide

생성물 1

HCID 205704722-Methyl-2-pinanylperoxy-4-pentanone수율 56.9%

반응 조건

온도
25 °C

실험 절차

A mixture of 11.8 g. (0.12 mole) of mesityl oxide and 25.40 g. (0.15 mole) of pinanyl hydroperoxide was stirred at 0° C. while 2.0 g. of 77% sulfuric acid solution was slowly added. The reaction mixture was allowed to warm slowly to 25° C. and stirred for a total of 16 hours. The organic layer was taken up in 30 ml. of either and washed with water, 5% sodium hydroxide solution and again with water to pH 8. The mixture was then subjected to steam distillation in the presence of sodium bicarbonate solution at 20 torr for 2 hours to remove unreacted mesityl oxide and pinanyl hydroperoxide. The product was taken up in ether, dried over anhydrous magnesium sulfate and the ether removed under reduced pressure leaving 18.14 g. of product (56.9% yield).

후처리

  1. additionA mixture of 11.8 g
  2. washof either and washed with water, 5% sodium hydroxide solution and again with water to pH 8
  3. distillationThe mixture was then subjected to steam distillation in the presence of sodium bicarbonate solution at 20 torr for 2 hours
  4. customto remove unreacted mesityl oxide and pinanyl hydroperoxide
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe ether removed under reduced pressure
  7. customleaving 18.14 g

출처 및 근거

ORD 기록
ord-2126ecab6e164cf49e90e9c1b1b4c7ca
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04289914

연결된 노트

불러오는 중…