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HCID 21191709、化合物 → Methyl 5-methoxy-2,3-dihydro-1H-indene-2-carboxylate

HRID 2069662
ノート
印刷プレビュー

反応式

HRID 2069662 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 21191709HCID 21191709、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 24247Perchloric Acid溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-09bcb48a9ca446df8b2440c764b00bb7
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08299117B2

反応ノート

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