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HCID 21191709, 화합물 → Methyl 5-methoxy-2,3-dihydro-1H-indene-2-carboxylate

HRID 1909574
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HRID 1909574 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[C:8](=O)[CH:7]([C:13]([O:15][CH3:16])=[O:14])[CH2:6]2>C(O)(=O)C.Cl(O)(=O)(=O)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[CH2:8][CH:7]([C:13]([O:15][CH3:16])=[O:14])[CH2:6]2
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참가 물질

4

반응물 1

HCID 21191709HCID 21191709, 화합물

생성물 1

HCID 53724337Methyl 5-methoxy-2,3-dihydro-1H-indene-2-carboxylate수율 46%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 24247Perchloric Acid용매

실험 절차

A mixture of methyl 5-methoxy-1-oxo-2,3-dihydro-1H-indene-2-carboxylate (5.5 g, 25 mmol) in acetic acid (0.64 M) and perchloric acid (14.9 M) was suspended in a pressure vessel and was shook under a hydrogen atmosphere (30 psi) for 4 hours. The mixture was filtered through a pad of celite and washed with chloroform. The organic phase was washed with water (5×) until the pH was neutral, followed with a wash with brine. The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was purified by silica gel chromatography (0-100% EtOAc in hexanes) to provide methyl 5-methoxy-2,3-dihydro-1h-indene-2-carboxylate (696) (46%).

후처리

  1. customwas suspended in a pressure vessel
  2. filtrationThe mixture was filtered through a pad of celite
  3. washwashed with chloroform
  4. washThe organic phase was washed with water (5×) until the pH
  5. washa wash with brine
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude material was purified by silica gel chromatography (0-100% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-bcba5693e1194888ba5bdd91a37b090a
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598374B2

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