Ethanol → HCID 66739083, 화합물

HRID 1641477

반응식

HRID 1641477 반응식
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]

참가 물질

6

반응물 5

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

생성물 1

HCID 66739083HCID 66739083, 화합물

반응 조건

온도
50 °C

실험 절차

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 concentratration 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.

후처리

  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. customThe resulting residue was purified by column chromatography (hexane:ethyl acetate=8:1)

출처 및 근거

ORD 기록
ord-dec84ba2ef56459b821ff2aa39e94f50
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08115014B2

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