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Water → HCID 19096637、化合物

HRID 1657206
ノート
印刷プレビュー

反応式

HRID 1657206 の反応式
C(O)[C@H]1O[C@H](O[C@]2(CO)O[C@H](CO)[C@@H](O)[C@@H]2O)[C@H](O)[C@@H](O)[C@@H]1O.O.[CH3:25][C:26]1([CH3:38])[O:31][C:30](=[O:32])[C:29]([CH2:33][CH2:34][C:35](=[O:37])[CH3:36])=[CH:28][O:27]1>C(OCC)(=O)C>[CH3:38][C:26]1([CH3:25])[O:31][C:30](=[O:32])[C:29]([CH2:33][CH2:34][CH:35]([OH:37])[CH3:36])=[CH:28][O:27]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 5988Sucrose2 回HCID 190966312,2-Dimethyl-5-(3-oxobutyl)-1,3-dioxin-4-one

生成物 1

HCID 19096637HCID 19096637、化合物収率 55%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
32 °C

実験手順

30 g of baker's yeast (made by Oriental Yeast Co., Ltd.) and 15 g of saccharose were added in 30 ml of tap water, and the solution was then stirred at 32° C. for 30 minutes. Afterward, 350 mg of 2,2-dimethyl-5-(3-oxobutyl)-1,3-dioxin-4-one were added thereto, and the solution was then stirred overnight at the same temperature. 7.5 g of saccharose were further added thereto, followed by stirring overnight. Water of the reaction solution was then distilled off under reduced pressure, and the resultant residue was extracted with dichloromethane and then dried over anhydrous sodium sulfate. Afterward, the solvent was distilled off, and the residue was then subjected to column chromatography (an eluent of hexane:ethyl acetate=4:1), thereby obtaining 161 mg (yield 55%) of (-)-2,2-dimethyl-5-(3-hydroxybutyl)-1,3-dioxin-4-one [a compound having the formula (1) in which n is 2, X is a hydrogen atom, Y is a hydrogen atom, and the substituent is present at the 5-position].

後処理

  1. stirringthe solution was then stirred overnight at the same temperature
  2. stirringby stirring overnight
  3. distillationWater of the reaction solution was then distilled off under reduced pressure
  4. extractionthe resultant residue was extracted with dichloromethane
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationAfterward, the solvent was distilled off

出典と根拠

ORDレコード
ord-a0c053cadc8a427497a7e1e1bde57736
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05256800

反応ノート

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