Ammonia → Chloridazon

HRID 848804

반응식

HRID 848804 반응식
[NH3:1].Cl[C:3]1[CH:4]=[N:5][N:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7](=[O:10])[C:8]=1[Cl:9].C1C(O)=CC=C(S(O)(=O)=O)C=1>>[NH2:1][C:3]1[CH:4]=[N:5][N:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7](=[O:10])[C:8]=1[Cl:9]

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 47654-Hydroxybenzenesulfonic acidHCID 728132-Phenyl-4,5-dichloro-3(2H)-pyridazinone

생성물 1

HCID 15546Chloridazon수율 89%

반응 조건

온도
130 °C

실험 절차

85 parts by volume of 15% (wt %) strength aqueous ammonia, 12.05 parts by weight of 4,5-dichloro-1-phenylpyridaz-6-one and 6.2 parts by weight of a 70% strength aqueous solution of phenol-4-sulfonic acid (parts by volume bearing the same relationship to parts by weight as the liter to the kilogram) are introduced into a jacketed pressure vessel having a capacity of 300 parts by volume. The reaction mixture is heated to 130° C. while stirring and kept for 4 hours at this temperature, while still stirring. The autogenous pressure which is hereupon generated is 6 bars. The reaction mixture is then allowed to cool to room temperature (20° C.) and the mother liquor is completely filtered off. The solid reaction product is washed with water and dried in vacuo at 100° C. There is obtained 9.8 parts by weight (89% of theory) of 4-amino-5-chloro-1-phenylpyridaz-6-one of melting point 205°-206° C. The amount of 5-amino-4-chloro-1-phenylpyridaz-6-one is determined gas-chromatographically and found to be 1%, and the amount of 4-amino derivative 99%.

후처리

  1. additionare introduced into a jacketed pressure vessel
  2. stirringwhile still stirring
  3. temperatureto cool to room temperature (20° C.)
  4. filtrationthe mother liquor is completely filtered off
  5. customThe solid reaction product
  6. washis washed with water
  7. customdried in vacuo at 100° C

출처 및 근거

ORD 기록
ord-0b7debef83af4415a9aef30002f5f67f
출처 데이터셋
uspto-grants-1981_10
특허 번호
US04297493

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