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

HRID 2181263

반응식

HRID 2181263 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f11a7298898f405b8052c69046015030
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06890959B2

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