Acetoxyacetyl chloride → 2-(Acetoxyacetylamino)-6-nitrobenzonitrile

HRID 2248761노트

반응식

HRID 2248761 반응식
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:3]=1[C:4]#[N:5].[C:13]([O:16][CH2:17][C:18](Cl)=[O:19])(=[O:15])[CH3:14]>N1C=CC=CC=1>[C:13]([O:16][CH2:17][C:18]([NH:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:3]=1[C:4]#[N:5])=[O:19])(=[O:15])[CH3:14]

참가 물질

4

반응물 2

HCID 26297Acetoxyacetyl chlorideHCID 127157292-Amino-6-nitrobenzonitrile

생성물 1

HCID 149862822-(Acetoxyacetylamino)-6-nitrobenzonitrile

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 2-amino-6-nitrobenzonitrile (6.5 g) in pyridine (100 ml) is cooled in an ice bath and thereto is added dropwise acetoxyacetyl chloride (4.4 ml). The mixture is stirred at room temperature for 1 hour, and thereafter, pyridine is distilled off under reduced pressure, and then water is added thereto, and the mixture is extracted with methylene chloride. The organic layer is washed with 1N hydrochloric acid and dried over anhydrous sodium sulfate, and the solvent is distilled off under reduced pressure. The resulting crude crystals are recrystallized from ethanol to give the title compound (5.8 g) having the following physical properties.

후처리

  1. distillationpyridine is distilled off under reduced pressure
  2. additionwater is added
  3. extractionthe mixture is extracted with methylene chloride
  4. washThe organic layer is washed with 1N hydrochloric acid
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent is distilled off under reduced pressure
  7. customThe resulting crude crystals are recrystallized from ethanol

출처 및 근거

ORD 기록
ord-6c0f96e5dae34bae80d214d5299054b8
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05041462

반응 노트

불러오는 중…