Ethanol → 130251-07-9

HRID 2194296ノート

反応式

HRID 2194296 の反応式
S(=O)(=O)(O)O.[Br:6][C@H:7]([CH2:11][CH3:12])[C:8]([OH:10])=[O:9].[CH2:13](O)[CH3:14]>>[Br:6][C@H:7]([CH2:11][CH3:12])[C:8]([O:10][CH2:13][CH3:14])=[O:9]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 6992738alpha-Bromobutyric acid, (R)-

生成物 1

HCID 7000062130251-07-9

実験手順

0.45 mL of sulfuric acid was added to ethanol (70 mL) solution of 7.0 g of (R)-2-bromobutyric acid at room temperature, and refluxed for 3 hours. The reaction mixture was cooled to room temperature, and poured into ice water (140 mL). The solution was extracted 3 times with ethyl acetate. The combined extract was sequentially washed with saturated sodium hydrogen carbonate solution and brine, and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated in vacuo, and 7.47 g of the subject compound was prepared as colorless oil. Optical purity 96% ee (HPLC)

後処理

  1. temperaturerefluxed for 3 hours
  2. extractionThe solution was extracted 3 times with ethyl acetate
  3. extractionThe combined extract
  4. washwas sequentially washed with saturated sodium hydrogen carbonate solution and brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationAfter filtration
  7. concentrationthe filtrate was concentrated in vacuo, and 7.47 g of the subject compound
  8. customwas prepared as colorless oil

出典と根拠

ORDレコード
ord-254f7db1dc424391b1abd5787be0b820
出典データセット
uspto-grants-2012_12
特許番号
US08329913B2

反応ノート

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