Ethanol → HCID 66739083、化合物

HRID 1908706

反応式

HRID 1908706 の反応式
Cl.[Br:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9]N.[C:11]([CH2:14][CH2:15][CH2:16][CH2:17][C:18]([OH:20])=[O:19])(=O)[CH3:12].S(=O)(=O)(O)O.C(=O)([O-])O.[Na+].[CH2:31](O)[CH3:32]>>[Br:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]2[C:4]=1[NH:9][C:11]([CH3:12])=[C:14]2[CH2:15][CH2:16][CH2:17][C:18]([O:20][CH2:31][CH3:32])=[O:19]

参加物

6

反応物 5

HCID 702EthanolHCID 1118Sulfuric AcidHCID 988106-Oxoheptanoic acidHCID 516892Sodium BicarbonateHCID 27239122-Bromophenylhydrazine hydrochloride

生成物 1

HCID 66739083HCID 66739083、化合物

反応条件

温度
50 °C

実験手順

To a solution of (2-bromophenyl)hydrazine hydrochloride (14 g) in ethanol (60 mL), 5-acetylvaleric acid (9.0 g) was added. The reaction mixture was stirred at 50° C. for 40 minutes, and concentrated sulfuric acid (6.0 mL) was added thereto, followed by heating under reflux for 16 hours. The reaction mixture was added to a saturated aqueous sodium hydrogen carbonate solution which was then extracted with ethyl acetate and dried over anhydrous sodium sulfate, followed by concentration under reduced pressure. The resulting residue was purified by column chromatography (hexane:ethyl acetate=8:1) to obtain the title compound (15 g) having the following physical properties.

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 16 hours
  3. extractionwas then extracted with ethyl acetate
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationfollowed by concentration under reduced pressure
  6. customThe resulting residue was purified by column chromatography (hexane:ethyl acetate=8:1)

出典と根拠

ORDレコード
ord-4295e18db1f149f794e3628bd88d7f26
出典データセット
uspto-grants-2013_12
特許番号
US08598223B2

関連ノート

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