Water → 4-(1-(4-(Aminosulfonyl)phenyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl)benzoic acid

HRID 2227401ノート

反応式

HRID 2227401 の反応式
[OH:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:13]([C:14]3[CH:19]=[CH:18][C:17]([S:20]([NH2:23])(=[O:22])=[O:21])=[CH:16][CH:15]=3)[N:12]=[C:11]([C:24]([F:27])([F:26])[F:25])[CH:10]=2)=[CH:5][CH:4]=1.CC(C)=[O:30].OS(O)(=O)=O.O=[Cr](=O)=O.C(OCC)(=O)C.O>CC(C)=O>[NH2:23][S:20]([C:17]1[CH:16]=[CH:15][C:14]([N:13]2[C:9]([C:6]3[CH:5]=[CH:4][C:3]([C:2]([OH:30])=[O:1])=[CH:8][CH:7]=3)=[CH:10][C:11]([C:24]([F:25])([F:26])[F:27])=[N:12]2)=[CH:19][CH:18]=1)(=[O:22])=[O:21]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 99087764'-HydroxycelecoxibHCID 131709961Jones' reagent

生成物 1

HCID 100472204-(1-(4-(Aminosulfonyl)phenyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl)benzoic acid

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To the product from Example 11 in 2 mL of acetone was added 1.33 M Jones reagent until an orange color persisted. The reaction was poured into 20 mL of ethyl acetate and 20 mL of H2O and the organic layer separated, washed with saturated sodium bisulfite and dried over MgSO4. The crude product was filtered through silica gel/Celite to afford the title compound as a yellow solid: HRMS m/z 411.0507 (calc'd for C17H12N3O4SF3, 411.0500).

後処理

  1. customthe organic layer separated
  2. washwashed with saturated sodium bisulfite
  3. dry with materialdried over MgSO4
  4. filtrationThe crude product was filtered through silica gel/Celite

出典と根拠

ORDレコード
ord-49a107c667d14665bd0dc21147884b04
出典データセット
uspto-grants-2002_07
特許番号
US06413960B1

反応ノート

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