Dichloromethane → 3,3-Dimethyl-1,5-dioxaspiro[5.5]undecan-8-one

HRID 2181263

反応式

HRID 2181263 の反応式
[C:1]1(=[O:8])[CH2:6][CH2:5][CH2:4][C:3](=[O:7])[CH2:2]1.[CH3:9][C:10]([CH3:15])([CH2:13]O)[CH2:11][OH:12].C(Cl)Cl.[OH-].[Na+]>C1(C)C=CC(S(O)(=O)=O)=CC=1.O>[CH3:9][C:10]1([CH3:15])[CH2:11][O:12][C:3]2([CH2:4][CH2:5][CH2:6][C:1](=[O:8])[CH2:2]2)[O:7][CH2:13]1

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 104341,3-CyclohexanedioneHCID 14798Sodium HydroxideHCID 31344Neopentyl glycol

生成物 1

HCID 153447493,3-Dimethyl-1,5-dioxaspiro[5.5]undecan-8-one収率 50%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 962Water溶媒

実験手順

448.5 g 1,3-cyclohexanedione, 416 g 2,2-dimethyl-1,3-propanediol and 12 g p-toluenesulfonic acid were introduced into 3,000 ml methylene chloride and the mixture was heated under reflux for 24 hours using a water separator. When the reaction had ended the mixture was cooled to room temperature and 2,000 ml 32% sodium hydroxide solution were added. The phases were separated and the organic phase was washed first with sodium bicarbonate solution (44.4 g sodium bicarbonate solution/850 ml water) and then with 350 ml water. The organic phase was dried over sodium sulfate and the solvent was then evaporated in vacuo. 345 g (50% of theory) 3,3-dimethyl-1,5-dioxa-spiro[5.5]undecan-8-one were obtained in this way.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 24 hours
  3. customThe phases were separated
  4. washthe organic phase was washed first with sodium bicarbonate solution (44.4 g sodium bicarbonate solution/850 ml water)
  5. dry with materialThe organic phase was dried over sodium sulfate
  6. customthe solvent was then evaporated in vacuo

出典と根拠

ORDレコード
ord-f11a7298898f405b8052c69046015030
出典データセット
uspto-grants-2005_05
特許番号
US06890959B2

関連ノート

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