Methanol → HCID 20542689, 화합물

HRID 2285979노트

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HRID 2285979 반응식
[C:1]1([N:7]2[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[C:10]([CH2:18][C:19]([OH:21])=[O:20])[C:9]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:28]O.S(=O)(=O)(O)O>C(Cl)(Cl)(Cl)Cl>[CH3:28][O:20][C:19](=[O:21])[CH2:18][C:10]1[C:9]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)=[N:8][N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:11]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 3084566Trifezolac

생성물 1

HCID 20542689HCID 20542689, 화합물수율 91%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

15 grams 1,3,5-triphenyl-pyrazol-4-acetic acid, 50 milliliters methanol, 40 milliliters carbon tetrachloride and 0.64 gram concentrated sulfuric acid were mixed and the mixture heated to the boiling temperature under reflux for 11 hours. The cooled reaction mixture was then extracted, first with sodium carbonate solution and thereafter with water. The organic phase was then dried and evaporated. The residue was recrystallized from a mixture of methanol and water. 14.2 grams 1,3,5-triphenylpyrazol-4-acetic acid-methyl ester, melting at 80.5°-81.5° C., were obtained, representing a yield of 91%.

후처리

  1. temperaturethe mixture heated to the boiling temperature
  2. temperatureunder reflux for 11 hours
  3. customThe cooled reaction mixture
  4. extractionwas then extracted, first with sodium carbonate solution
  5. customThe organic phase was then dried
  6. customevaporated
  7. customThe residue was recrystallized from a mixture of methanol and water

출처 및 근거

ORD 기록
ord-3066bb22df1f4180bb96bb7a92190eb9
출처 데이터셋
uspto-grants-1982_04
특허 번호
US04325962

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