Water → HCID 178463110、化合物

HRID 1276128

反応式

HRID 1276128 の反応式
[C:1](=[O:4])([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:23]([C:24]2[N:28]([CH3:29])[N:27]=[C:26]([C:30]([CH3:32])=[O:31])[CH:25]=2)=[C:22]([Cl:33])[CH:21]=[CH:20][C:9]=1[C:10]([O:12]C1N(CC)N=CC=1)=O.O>O1CCOCC1>[Cl:7][C:8]1[C:23]([C:24]2[N:28]([CH3:29])[N:27]=[C:26]([C:30]([CH3:32])=[O:31])[CH:25]=2)=[C:22]([Cl:33])[CH:21]=[CH:20][C:9]=1[C:10]([C:25]1[CH:26]=[N:27][N:28]([CH2:24][CH3:23])[C:1]=1[OH:4])=[O:12]

参加物

5

反応物 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 53727367(1-ethylpyrazol-5-yl) 2,4-dichloro-3-(1-methyl-3-methylcarbonyl-1H-pyrazol-5-yl)benzoate

生成物 1

HCID 178463110HCID 178463110、化合物収率 135.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

0.076 g (0.6 mmol) of potassium carbonate was added to 0.16 g (0.4 mmol) of (1-ethylpyrazol-5-yl) 2,4-dichloro-3-(1-methyl-3-methylcarbonyl-1H-pyrazol-5-yl)benzoate in 3 ml of dioxane and the mixture was heated under reflux for 3 hours and then stirred at room temperature for 12 hours. 50 ml of water were added, the solution was washed with methylene chloride and methyl t-butyl ether, nitrogen was passed through and the pH was adjusted to 1 using 10% strength hydrochloric acid. The precipitate that had formed was filtered off with suction, washed with water and taken up in ethyl acetate. After drying, this organic phase was concentrated. 0.11 g (69% of theory) of 4-[2,4-dichloro-3-(1-methyl-3-methylcarbonyl-1H-pyrazol-5-yl)benzoyl]-1-ethyl-5-hydroxy-1H-pyrazole was obtained.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. washthe solution was washed with methylene chloride and methyl t-butyl ether, nitrogen
  4. customThe precipitate that had formed
  5. filtrationwas filtered off with suction
  6. washwashed with water
  7. customAfter drying
  8. concentrationthis organic phase was concentrated

出典と根拠

ORDレコード
ord-e66cd86e9bf546feaafb03fc65e078f9
出典データセット
uspto-grants-2000_12
特許番号
US06165944

関連ノート

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