反応 #1552093

ord-cd43efc8cabb426faecfce1625f25ae6

反応方程式

O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
CC(C)(C)CCC1CCCC1=O
2-(3,3-dimethylbutyl)cyclopentanone
Cl.NO
hydroxylamine hydrochloride
CC(C)(C)CCC1CCCC1=NO
2-(3,3-dimethylbutyl)-N-hydroxycyclopentanimine

溶媒

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture is cooled to room temperature
  2. 2
    ろ過filtered off
  3. 3
    濃縮the product is concentrated under reduced pressure
  4. 4
    抽出The residue is extracted with water/diethyl ether
  5. 5
    乾燥phase is dried with sodium sulphate
  6. 6
    濃縮concentrated under reduced pressure

実験手順

At 0° C., aq. sodium carbonate solution is added to a solution consisting of 20.0 g of (119 mmol) of 2-(3,3-dimethylbutyl)cyclopentanone and 16.5 g (238 mmol) of hydroxylamine hydrochloride in 200 ml of methanol until the pH is 8. The mixture is then stirred at 50° C. for 15 hours. After the reaction has ended, the mixture is cooled to room temperature and filtered off and the product is concentrated under reduced pressure. The residue is extracted with water/diethyl ether. The org. phase is dried with sodium sulphate and concentrated under reduced pressure. This gives 20.0 g (92% of theory) of an 2-(3,3-dimethylbutyl)-N-hydroxycyclopentanimine.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08999956B2uspto-grants-2015_04