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

HRID 1527266노트

반응식

HRID 1527266 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 21265856HCID 21265856, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-7e0f640545b045ebaa3929d2bf9f0a96
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085555B2

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