Methanol → HCID 20542689、化合物

HRID 2285979ノート

反応式

HRID 2285979 の反応式
[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

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 3084566Trifezolac

生成物 1

HCID 20542689HCID 20542689、化合物収率 91%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-3066bb22df1f4180bb96bb7a92190eb9
出典データセット
uspto-grants-1982_04
特許番号
US04325962

反応ノート

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