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Hydrochloric Acid → HCID 178434075, 화합물

HRID 1980376
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HRID 1980376 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 178434075HCID 178434075, 화합물수율 69.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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%

후처리

  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

출처 및 근거

ORD 기록
ord-722a9ab71bf24b7d8d804809d7691824
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04508910

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