Hydrochloric Acid → 3-Methyl-4-(2-pyridylazo)-1-(p-sulfophenyl)-2-pyrazolin-5-one

HRID 261454노트

반응식

HRID 261454 반응식
Br[C:2]1(Br)[C:6](=[O:7])[N:5]([C:8]2[CH:13]=[CH:12][C:11]([S:14]([OH:17])(=[O:16])=[O:15])=[CH:10][CH:9]=2)[N:4]=[C:3]1[CH3:18].[NH:20]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)[NH2:21].Cl>O>[CH3:18][C:3]1[CH:2]([N:21]=[N:20][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=2)[C:6](=[O:7])[N:5]([C:8]2[CH:13]=[CH:12][C:11]([S:14]([OH:17])(=[O:16])=[O:15])=[CH:10][CH:9]=2)[N:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 786452-HydrazinopyridineHCID 203940744,4-Dibromo-3-methyl-1-(4-sulfophenyl)-2-pyrazolin-5-one

생성물 1

HCID 203940703-Methyl-4-(2-pyridylazo)-1-(p-sulfophenyl)-2-pyrazolin-5-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

41.0 g (0.10 mole) of 4,4-dibromo-3-methyl-1-(4-sulfophenyl)-2-pyrazolin-5-one, which can be prepared according to the method of Machiele, U.S. Pat. No. 3,952,009 (Example 1), and 16.0 g (0.15 mole) of 2-hydrazinopyridine were combined in 180 ml of water. The mixture was heated on the steam bath a total of six hours. After a few minutes of heating, the solution goes to a very thick slurry. The mixture was cooled somewhat, 10 ml of concentrated HCl were added, and the orange solid was isolated by suction filtration. After washing once with tetrahydrofuran, twice with ether, and drying, the yield of dye was 17.8 g (50 percent).

후처리

  1. temperatureThe mixture was heated on the steam bath a total of six hours
  2. temperatureAfter a few minutes of heating
  3. temperatureThe mixture was cooled somewhat
  4. customthe orange solid was isolated by suction filtration
  5. washAfter washing once with tetrahydrofuran, twice with ether
  6. customdrying

출처 및 근거

ORD 기록
ord-c120b587ee2b4627ab4f1606da65dd17
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04165987

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