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Hydrochloric Acid → HCID 178434075、化合物

HRID 614954
ノート
印刷プレビュー

反応式

HRID 614954 の反応式
[CH3:1][N:2]1[C:6](=[O:7])[CH:5]=[C:4]([CH3:8])[NH:3]1.[OH-].[Ca+2].[OH-].[N+:12]([C:15]1[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=1)([O-:14])=[O:13].Cl>O1CCOCC1>[CH3:1][N:2]1[C:6]([OH:7])=[C:5]([C:19](=[O:20])[C:18]2[CH:17]=[CH:16][C:15]([N+:12]([O-:14])=[O:13])=[CH:23][CH:22]=2)[C:4]([CH3:8])=[N:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 85024-Nitrobenzoyl chlorideHCID 27668471,3-dimethyl-1H-pyrazol-5-olHCID 6093208Calcium Hydroxide

生成物 1

HCID 178434075HCID 178434075、化合物収率 69.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

In 22 ml. of dry dioxane is dissolved 2.24 g. of 1,3-dimethyl-5-pyrazolone and then 2.96 g. of calcium hydroxide is added thereto. 3.71 g. of p-nitrobenzoyl chloride is added dropwise thereto while stirring at room temperature. After completion of the dropwise addition, the mixture is heated under reflux for 1 hour. After completion of the reaction, the reaction mixture is allowed to cool and then 40 ml. of a 2N hydrochloric acid solution is added thereto. Crystalline substances thus separated are recovered by filtration and washed with water to give 4.38 g. of crude crystals. This product is recrystallized from methanol to give 3.62 g. of the desired product as pale yellow columns having a melting point of 234°-235° C. Yield 69.3%

後処理

  1. additionAfter completion of the dropwise addition
  2. temperaturethe mixture is heated
  3. temperatureunder reflux for 1 hour
  4. customAfter completion of the reaction
  5. temperatureto cool
  6. customCrystalline substances thus separated
  7. filtrationare recovered by filtration
  8. washwashed with water
  9. customto give 4.38 g
  10. customThis product is recrystallized from methanol
  11. customto give 3.62 g

出典と根拠

ORDレコード
ord-bc9e4b4a50b9435298c3b553a3e11948
出典データセット
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04146726

反応ノート

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