Dimethylamine → 6-(Dimethylamino)pyrimidine-4-carboxylic acid

HRID 614378

반응식

HRID 614378 반응식
[C:1]([C:4]1[CH:9]=[C:8](Cl)[N:7]=[CH:6][N:5]=1)([OH:3])=[O:2].[CH3:11][NH:12][CH3:13]>>[C:1]([C:4]1[CH:9]=[C:8]([N:12]([CH3:13])[CH3:11])[N:7]=[CH:6][N:5]=1)([OH:3])=[O:2]

참가 물질

3

반응물 2

HCID 674DimethylamineHCID 166377476-Chloro-4-pyrimidinecarboxylic acid

생성물 1

HCID 213291656-(Dimethylamino)pyrimidine-4-carboxylic acid

실험 절차

A 40% aqueous dimethylamine solution (2000 cc) is added to 4-carboxy-6-chloropyrimidine (93.6 g). The mixture is allowed to stand for 3 days and then concentrated to dryness under reduced pressure. The residue is dissolved in water (300 cc). The solution is made alkaline by the addition of sodium bicarbonate powder to a pH of 8 to 9. The solution is then extracted with diisopropyl ether (1000 cc). The aqueous phase is acidified with 12N hydrochloric acid to a pH of 2 to 3. The precipitate is filtered off, washed with ice-water (30 cc) and then with isopropanol (120 cc). 4-Carboxy-6-dimethylaminopyrimidine (73.6 g), melting at 250° C., is obtained.

후처리

  1. concentrationconcentrated to dryness under reduced pressure
  2. dissolutionThe residue is dissolved in water (300 cc)
  3. additionby the addition of sodium bicarbonate powder to a pH of 8 to 9
  4. extractionThe solution is then extracted with diisopropyl ether (1000 cc)
  5. filtrationThe precipitate is filtered off
  6. washwashed with ice-water (30 cc)

출처 및 근거

ORD 기록
ord-46ae30d71bd24b698c12d1a16fd14953
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144339

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