Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- → HCID 21265856、化合物

HRID 1527266ノート

反応式

HRID 1527266 の反応式
[CH:1]1[N:2]=[C:3]([CH2:10][C:11]([OH:13])=[O:12])[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.[C:14]12(CS(O)(=O)=O)C(C)(C)C(CC1)CC2=O>CO>[CH3:14][O:12][C:11](=[O:13])[CH2:10][C:3]1[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]2=[CH:1][N:2]=1

参加物

4

反応物 2

HCID 18462Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-HCID 55262594HCID 55262594、化合物

生成物 1

HCID 21265856HCID 21265856、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A suspension of imidazo[1,5-a]pyridin-3-ylacetic acid (Ellanovalabs, 2 g, 11.35 mmol) and camphorsulfonic acid (2.9 g, 12.49 mmol) in MeOH (120 mL) was refluxed for 4 h. Then allowed to cool to RT and concentrated under reduced pressure. The crude residue was diluted in CH2Cl2 and the organic layer was washed with a saturated aqueous solution of NaHCO3. The organics were dried (Na2SO4), filtered and concentrated. The material thus obtained was used in the next step without further purification: TLC, Rf (CH2Cl2/MeOH 9:1)=0.55; MS (UPLC/MS): 191.1 [M+H]+; tR (HPLC conditions f): 0.4 min.

後処理

  1. temperaturewas refluxed for 4 h
  2. concentrationconcentrated under reduced pressure
  3. additionThe crude residue was diluted in CH2Cl2
  4. washthe organic layer was washed with a saturated aqueous solution of NaHCO3
  5. dry with materialThe organics were dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe material thus obtained
  9. customwas used in the next step without further purification
  10. custom0.4 min.

出典と根拠

ORDレコード
ord-7e0f640545b045ebaa3929d2bf9f0a96
出典データセット
uspto-grants-2015_07
特許番号
US09085555B2

反応ノート

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