Sodium Hydroxide → 4,4,5,8-Tetramethyl-1-oxaspiro[2.5]octane

HRID 2051369ノート

反応式

HRID 2051369 の反応式
[OH-].[Na+].[CH3:3][C:4]1([CH3:13])[CH:9]([CH3:10])[CH2:8][CH2:7][CH:6]([CH3:11])[C:5]1=[O:12].[Cl-].[CH3:15][S+](C)C>CS(C)=O>[CH3:13][C:4]1([CH3:3])[CH:9]([CH3:10])[CH2:8][CH2:7][CH:6]([CH3:11])[C:5]21[O:12][CH2:15]2

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 51304442,2,3,6-TetramethylcyclohexanoneHCID 10176118Trimethylsulfonium chloride

生成物 1

HCID 187910594,4,5,8-Tetramethyl-1-oxaspiro[2.5]octane

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

According to a preferred embodiment of the invention, NaOH is added to a mixture consisting of 2,2,3,6-tetramethyl-1-cyclohexanone and trimethylsulfonium chloride in dimethylsulfoxide. The reaction is slightly exothermic, hence the necessity to maintain an external cooling of the reaction mixture so as to keep the temperature at about 25°-30° C. Good stirring is also applied for about 6 hr. 4,4,5,8-Tetramethyl-1-oxaspiro[2.5]octane is then obtained by extraction of the resulting mixture with petrol ether, concentration of the organic extracts and fractional distillation.

後処理

  1. additionis added to a mixture
  2. temperaturehence the necessity to maintain
  3. temperaturean external cooling of the reaction mixture so as
  4. customat about 25°-30° C

出典と根拠

ORDレコード
ord-f85b611f44f54e56bd406f3464041f72
出典データセット
uspto-grants-1991_05
特許番号
US05017711

反応ノート

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