Methyl acetoacetate → HCID 10192605、化合物

HRID 548774ノート

反応式

HRID 548774 の反応式
[C:1]([O:7]C)(=O)[CH2:2][C:3]([CH3:5])=O.Cl.[CH:10]1([NH:16][NH2:17])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1.[OH-].[Na+]>>[CH:10]1([N:16]2[C:1](=[O:7])[CH2:2][C:3]([CH3:5])=[N:17]2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1

参加物

4

反応物 3

HCID 7757Methyl acetoacetateHCID 14798Sodium HydroxideHCID 207836Cyclohexylhydrazine hydrochloride

生成物 1

HCID 10192605HCID 10192605、化合物収率 79%

実験手順

A mixture solution of 14.5 mL (0.134 mol) of methyl acetoacetate and 20.2 g (0.134 mol) of cyclohexylhydrazine hydrochloride was stirred for 2 hours at 120° C., and the mixture was cooled. Then, the reaction mixture was neutralized with 30 mL of 4M-sodium hydroxide solution and extracted with ethyl acetate. The organic layer was washed with water and saturated saline solution and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the resulting residue was treated with hexane. The resulting precipitate was collected to give 19.0 g (79%) of the titled compound.

後処理

  1. temperaturethe mixture was cooled
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated saline solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. additionthe resulting residue was treated with hexane
  7. customThe resulting precipitate was collected

出典と根拠

ORDレコード
ord-b194eb098e3b423a8f628346149c4b74
出典データセット
uspto-grants-2011_05
特許番号
US07943624B2

反応ノート

読み込み中…