Acetic Anhydride → HCID 67199459、化合物

HRID 551668ノート

反応式

HRID 551668 の反応式
O[CH:2]([CH2:8][CH2:9][CH:10]=[CH2:11])[CH:3]([CH3:7])[C:4]([OH:6])=O.C([O-])(=O)C.[K+].C(OC(=O)C)(=O)C>C(OCC)(=O)C>[CH3:7][C@@:3]12[C:4](=[O:6])[CH2:11][C@@H:10]1[CH2:9][CH:8]=[CH:2]2

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 517044Potassium AcetateHCID 14924162HCID 14924162、化合物

生成物 1

HCID 67199459HCID 67199459、化合物収率 19.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixed solution of 3-hydroxy-2-methylhept-6-enoic acid (5.45 g, 34.5 mmol), potassium acetate (7.0 g, 71.3 mmol), and acetic anhydride (30 mL) was stirred at room temperature for 1.5 hours and then stirred for 3 hours under conditions of heating to reflux. The reaction solution was left overnight, then diluted with ethyl acetate, washed with water, saturated aqueous sodium bicarbonate, and saturated saline, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the obtained residue was purified by silica gel column chromatography to obtain the compound of interest as a pale yellow oil (810 mg).

後処理

  1. temperatureof heating to reflux
  2. waitThe reaction solution was left overnight
  3. washwashed with water, saturated aqueous sodium bicarbonate, and saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-1b70956e1f8d4004a6c914cdc674b12a
出典データセット
uspto-grants-2011_05
特許番号
US07947738B2

反応ノート

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