Sodium Hydroxide → 2,2,N-Trimethyl-N-(4-oxocyclohexyl)propionamide

HRID 1748614노트

반응식

HRID 1748614 반응식
O1[C:5]2([CH2:10][CH2:9][CH:8]([N:11]([CH3:18])[C:12](=[O:17])[C:13]([CH3:16])([CH3:15])[CH3:14])[CH2:7][CH2:6]2)[O:4]CC1.[OH-].[Na+]>Cl>[CH3:14][C:13]([CH3:16])([CH3:15])[C:12]([N:11]([CH3:18])[CH:8]1[CH2:9][CH2:10][C:5](=[O:4])[CH2:6][CH2:7]1)=[O:17]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 79111757N-(1,4-Dioxaspiro[4,5]dec-8-yl)-2,2,N-trimethylpropionamide

생성물 1

HCID 791196402,2,N-Trimethyl-N-(4-oxocyclohexyl)propionamide수율 70.1%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

To N-(1,4-dioxaspiro[4,5]dec-8-yl)-2,2,N-trimethylpropionamide (12.5 g) was added 6 N hydrochloric acid aqueous solution (50 ml), and stirred at room temperature for 1 hour. After completion of the reaction, 12 N aqueous solution of sodium hydroxide (25 ml) was added thereto, and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and then the solvent was evaporated. To the obtained residue was added diisopropyl ether, the insoluble matter was collected by filtration, and then dried to give the titled compound (7.25 g) as a white solid. MS (ESI) m/z: 212 (M+H)+.

후처리

  1. additionwas added
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. customthe solvent was evaporated
  5. additionTo the obtained residue was added diisopropyl ether
  6. filtrationthe insoluble matter was collected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-46e9cf22ab3d4654993d995afa42fd7b
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09150555B2

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