Trichloroacetyl chloride → 2-(2-Trichloroacetylpyrrol-1-yl)malonic acid diethyl ester

HRID 256586

반응식

HRID 256586 반응식
[CH2:1]([O:3][C:4](=[O:16])[CH:5]([N:11]1[CH:15]=[CH:14][CH:13]=[CH:12]1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2].[Cl:17][C:18]([Cl:23])([Cl:22])[C:19](Cl)=[O:20]>C(Cl)(Cl)Cl>[CH2:9]([O:8][C:6](=[O:7])[CH:5]([N:11]1[CH:12]=[CH:13][CH:14]=[C:15]1[C:19](=[O:20])[C:18]([Cl:23])([Cl:22])[Cl:17])[C:4]([O:3][CH2:1][CH3:2])=[O:16])[CH3:10]

참가 물질

4

반응물 2

HCID 6420Trichloroacetyl chlorideHCID 2782128diethyl 2-(1H-pyrrol-1-yl)malonate

생성물 1

HCID 105471632-(2-Trichloroacetylpyrrol-1-yl)malonic acid diethyl ester수율 89%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 2-(pyrrol-1-yl)malonic acid diethyl ester (100.0 g) in chloroform (100 ml) was added trichloroacetyl chloride (161.4 g), and the resulting mixture was refluxed for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate. The solution was washed with 10% aqueous sodium carbonate solution and then with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and evaporated under reduced pressure. The residue was recrystallized from isopropyl ether to give the title compound (146.4 g, 89.0%) as colorless crystals, mp 67°-69° C.

후처리

  1. temperaturethe resulting mixture was refluxed for 15 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe solution was washed with 10% aqueous sodium carbonate solution
  5. dry with materialwith saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate
  6. customevaporated under reduced pressure
  7. customThe residue was recrystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-fb9e6de47aa948b9b0384c1ba25e19a7
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258382

연결된 노트

불러오는 중…