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

HRID 1748614ノート

反応式

HRID 1748614 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-46e9cf22ab3d4654993d995afa42fd7b
出典データセット
uspto-grants-2015_10
特許番号
US09150555B2

反応ノート

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