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

HRID 127861

反応式

HRID 127861 の反応式
[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]

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 8858Mesityl oxideHCID 147175701-Pinanyl hydroperoxide

生成物 1

HCID 205704722-Methyl-2-pinanylperoxy-4-pentanone収率 56.9%

反応条件

温度
25 °C

実験手順

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 ether 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).

後処理

  1. additionA mixture of 11.8 g
  2. washof ether 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

出典と根拠

ORDレコード
ord-75a878b802034342af05cac37840b8a4
出典データセット
uspto-grants-1981_03
特許番号
US04257985

関連ノート

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