Dimethylformamide → HCID 57780058, 화합물

HRID 251973노트

반응식

HRID 251973 반응식
P(Cl)(Cl)(Cl)=O.[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:8]=1[N:14]1[CH:18]=[CH:17][CH:16]=[CH:15]1.[OH-].[Na+].CN(C)[CH:23]=[O:24]>>[Cl:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([Cl:6])[C:8]=1[N:14]1[CH:18]=[CH:17][CH:16]=[C:15]1[CH:23]=[O:24]

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 207882021-(2,6-Dichlorophenyl)-1H-pyrrole

생성물 1

HCID 57780058HCID 57780058, 화합물수율 33.7%

실험 절차

Under ice-cooling, 7.67 g of phosphorus oxychloride was added dropwise to 4 g of N,N-dimethylformamide. The mixture was stirred at room temperature for 30 minutes, and 2.1 g of 1-(2,6-dichlorophenyl)-1H-pyrrole was added thereto. The resulting mixture was stirred at 60° C. for 2 hours, allowed to cool to room temperature, and then poured into ice water. The mixture was adjusted to pH 4 by an addition of a 2N aqueous sodium hydroxide solution, and then extracted with ethyl acetate two times. The organic layers were combined, washed successively with water and an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel chromatography to obtain 0.80 g of 1-(2,6-dichlorophenyl)-1H-pyrrole-2-carbaldehyde of the formula:

후처리

  1. temperatureUnder ice-cooling
  2. stirringThe resulting mixture was stirred at 60° C. for 2 hours
  3. temperatureto cool to room temperature
  4. extractionextracted with ethyl acetate two times
  5. washwashed successively with water
  6. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-cdefac832a4b4342a98d6d2e5f90dbe5
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07867949B2

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