反応 #571855

ord-bc022da9e4834b498fc58523de2ad1c9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度chilled to -5° to -10° C
  2. 2
    その他rises to 26° C
  3. 3
    洗浄The mixture is washed with ether
  4. 4
    抽出extracted with ethyl acetate (two times)
  5. 5
    乾燥The combined extracts are dried over sodium sulfate
  6. 6
    濃縮concentrated under reduced pressure until crystalline solids
  7. 7
    その他form
  8. 8
    その他the crystals are collected (34.8 g)

実験手順

L-Threonine (35.7 g) is dissolved in 1N sodium hydroxide (1 liter) and chilled to -5° to -10° C. To the cold, mechanically stirred solution is added dropwise phenylacetyl chloride (46.3 g). The reaction mixture is stirred for about 16 hours as the temperature rises to 26° C. The mixture is washed with ether, acidified to pH 2 with hydrochloric acid, and extracted with ethyl acetate (two times). The combined extracts are dried over sodium sulfate and concentrated under reduced pressure until crystalline solids form. Ether is added to the mixture and the crystals are collected (34.8 g); melting point 161°-163° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04533660uspto-grants-1985_08