Trifluoroacetic acid → HCID 178506540、化合物

HRID 910243ノート

反応式

HRID 910243 の反応式
[I:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:10]3[CH:15]=[CH:14][C:13]([C:16]4[CH:20]=[CH:19][N:18](C(OC(C)(C)C)=O)[N:17]=4)=[CH:12][CH:11]=3)=[N:7][C:6]=2[CH:28]=1.FC(F)(F)C(O)=O>C(Cl)(Cl)Cl>[I:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:10]3[CH:11]=[CH:12][C:13]([C:16]4[CH:20]=[CH:19][NH:18][N:17]=4)=[CH:14][CH:15]=3)=[N:7][C:6]=2[CH:28]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 67405262HCID 67405262、化合物

生成物 1

HCID 178506540HCID 178506540、化合物収率 84.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Subsequently, tert-butyl 3-[4-(5-iodo-1,3-benzoxazol-2-yl)phenyl]-1H-1-pyrazolecarboxylate (14.6 mg) was dissolved in chloroform (500 μL), and trifluoroacetic acid (231 μL) was added to the solution, followed by stirring at room temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, followed by drying. The thus-obtained white solid was dissolved in chloroform, and the solution was washed sequentially with 1N aqueous sodium hydroxide, water, and saturated saline, followed by drying over magnesium sulfate. The solvent was evaporated under reduce pressure, and the solid was recovered through filtration by use of isopropyl ether, followed by drying under reduced pressure, to thereby yield the title compound (9.8 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customby drying
  3. dissolutionThe thus-obtained white solid was dissolved in chloroform
  4. washthe solution was washed sequentially with 1N aqueous sodium hydroxide, water, and saturated saline
  5. dry with materialby drying over magnesium sulfate
  6. customThe solvent was evaporated
  7. filtrationthe solid was recovered through filtration by use of isopropyl ether
  8. customby drying under reduced pressure

出典と根拠

ORDレコード
ord-cb9f05a5b750475c8f67e37817362ea1
出典データセット
uspto-grants-2011_09
特許番号
US08022075B2

反応ノート

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