Perchloric Acid → (7-methyl-1H-indazol-5-yl)-acetaldehyde

HRID 2099735

반응식

HRID 2099735 반응식
C[O:2][CH:3]=[CH:4][C:5]1[CH:6]=[C:7]2[C:11](=[C:12]([CH3:14])[CH:13]=1)[NH:10][N:9]=[CH:8]2.Cl(O)(=O)(=O)=O>O1CCCC1.O.C(OCC)(=O)C>[CH3:14][C:12]1[CH:13]=[C:5]([CH2:4][CH:3]=[O:2])[CH:6]=[C:7]2[C:11]=1[NH:10][N:9]=[CH:8]2

참가 물질

6

반응물 2

HCID 24247Perchloric Acid2회HCID 690713565-(2-methoxy-vinyl)-7-methyl-1H-indazole

생성물 1

HCID 57794606(7-methyl-1H-indazol-5-yl)-acetaldehyde

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 5-(2-methoxy-vinyl)-7-methyl-1H-indazole (365 mg, 1.94 mmol, 1.0 equiv.) in tetrahydrofuran (8 mL) was added 60% perchloric acid (0.63 mL, 3 equiv) in one portion under nitrogen. After 2 h, more perchloric acid (0.63 mL) was added. After 4 h, LCMS indicated that no starting material was present. The reaction mixture was diluted with water and ethyl acetate. The layers were separated and the organic layer was washed with water (3×). The organic layer was separated, dried over sodium sulfate and concentrated in vacuo to give an off-white solid. The crude material was carried on without further purification. MS (ESI) [M+H]+=175.

후처리

  1. waitAfter 4 h
  2. customThe layers were separated
  3. washthe organic layer was washed with water (3×)
  4. customThe organic layer was separated
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customto give an off-white solid
  8. customThe crude material was carried on without further purification

출처 및 근거

ORD 기록
ord-ecfc209e6f2d414c95bff7906908e453
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07569578B2

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