Acetic Acid → Diclomezine

HRID 746275

반응식

HRID 746275 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:10](=O)[CH2:11][CH:12](OC)[C:13]([O:15]C)=O)[CH:5]=[C:6]([Cl:9])[C:7]=1[CH3:8].C(O)(=O)C.O.[NH2:25][NH2:26]>O>[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2[CH:11]=[CH:12][C:13](=[O:15])[NH:25][N:26]=2)[CH:5]=[C:6]([Cl:9])[C:7]=1[CH3:8]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 23310759HCID 23310759, 화합물

생성물 1

HCID 93341Diclomezine수율 86.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.53 g (0.005 mole) of methyl 4-(3,5-dichloro-4-methylphenyl)-2-methoxy-4-oxobutyrate were added to 4 ml of acetic acid and the mixture was heated to form a solution, to which was then added 0.275 g (0.0055 mole) of hydrazine monohydrate. The mixture was heated under reflux for 3 hours and then cooled, after which it was diluted with 40 ml of water and stirred. The resulting crystals were collected by filtration, washed successively with water and with a small amount of ethyl acetate and then air-dried, to give 1.1 g (yield 86.2%) of the desired 6-(3,5-dichloro-4-methylphenyl)-3(2H)pyridazinone, having properties the same as those of the preceding Examples.

후처리

  1. temperaturethe mixture was heated
  2. customto form a solution
  3. temperatureThe mixture was heated
  4. temperatureunder reflux for 3 hours
  5. temperaturecooled
  6. filtrationThe resulting crystals were collected by filtration
  7. washwashed successively with water and with a small amount of ethyl acetate
  8. customair-dried

출처 및 근거

ORD 기록
ord-89ae42bfb8c24ff489fae5fa387abecb
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04603201

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