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Trifluoroacetic acid → HCID 136339895、化合物

HRID 81411
ノート
印刷プレビュー

反応式

HRID 81411 の反応式
[C:1]1([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:6]=[CH:5][C:4]([CH2:7][N:8]2[CH:16]=[C:15]3[C:10]([N:11](CC4C=CC(OC)=CC=4)[C:12](=[O:19])[N:13]([CH3:18])[C:14]3=[O:17])=[N:9]2)=[CH:3][CH:2]=1.C(O)(C(F)(F)F)=O.FC(F)(F)S(O)(=O)=O>C(Cl)Cl>[C:1]1([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:2]=[CH:3][C:4]([CH2:7][N:8]2[CH:16]=[C:15]3[C:10]([NH:11][C:12](=[O:19])[N:13]([CH3:18])[C:14]3=[O:17])=[N:9]2)=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 68507378HCID 68507378、化合物

生成物 1

HCID 136339895HCID 136339895、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(biphenyl-4-ylmethyl)-7-(4-methoxybenzyl)-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione in CH2Cl2 (90 mL) is added TFA (10 mL) slowly at room temperature, followed by adding trifluoromethanesulfonic acid (4 mL) dropwise. After the reaction mixture is stirred at r.t. for 3 hours, solvent is removed under reduced pressure, and the obtained residue is basified by adding cold pre-diluted ammonium hydroxide (NH3 content, 7%) at 0° C. The mixture is extracted with ethyl acetate four times. The combined organic phase is washed with brine, dried over anhydrous Na2SO4, and then filtered. The filtrate is evaporated to dryness to give crude product in almost quantitative yield. MS (ESI) m/z 333.1 [M+H]+.

後処理

  1. customsolvent is removed under reduced pressure
  2. additionby adding cold pre-diluted ammonium hydroxide (NH3 content, 7%) at 0° C
  3. extractionThe mixture is extracted with ethyl acetate four times
  4. washThe combined organic phase is washed with brine
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. customThe filtrate is evaporated to dryness
  8. customto give crude product in almost quantitative yield

出典と根拠

ORDレコード
ord-eba80dccf1a642aa855391726adce802
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846693B2

反応ノート

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