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Dimethylformamide → 4-Dimethylamino-2-nitrobenzaldehyde

HRID 918553
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인쇄 미리보기

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HRID 918553 반응식
P(Cl)(Cl)(Cl)=O.[N+:6]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[N:12]([CH3:14])[CH3:13])([O-:8])=[O:7].CN(C)[CH:20]=[O:21]>>[N+:6]([C:9]1[CH:10]=[C:11]([N:12]([CH3:13])[CH3:14])[CH:15]=[CH:16][C:17]=1[CH:20]=[O:21])([O-:8])=[O:7]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 69269N,N-Dimethyl-3-nitroaniline

생성물 1

HCID 2913524-Dimethylamino-2-nitrobenzaldehyde수율 66%

반응 조건

온도
80 °C

실험 절차

720 parts of phosphorus oxychloride is added at 25°C to a solution of 498 parts of m-nitrodimethylaniline in 1800 parts by volume of dimethylformamide. The mixture is then heated within 1 hour to 75° to 80°C and stirred at this temperature for six hours. After the solution has cooled it is poured into 6000 parts of ice-water. The precipitate is suction filtered, washed and recrystallized from acetone. 385 parts (66% of theory) of 2-nitro-4-dimethylaminobenzaldehyde having a melting point of 115° to 116°C is obtained. ##SPC14##

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후처리

  1. temperatureAfter the solution has cooled it
  2. filtrationfiltered
  3. washwashed
  4. customrecrystallized from acetone

출처 및 근거

ORD 기록
ord-d34ef8ca76e045609c7476aab3f3ae63
출처 데이터셋
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03971821

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