反応 #4634

ord-b83de7ddf3984ec7810453a88a6980b1

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The solids are then suction-filtered whilst hot,
  2. 2
    洗浄washed with acetonitrile
  3. 3
    濃縮the filtrate is concentrated by evaporation in vacuo
  4. 4
    その他The oil remaining crystallises when
  5. 5
    workup.WAITleft
  6. 6
    その他is recrystallised from 320 ml of ethyl acetate, with carbon treatment

実験手順

A mixture of 29.2 g of N-(2-hydroxyethyl)-N'-(2-hydroxybenzyl)urea, 440 ml of epichlorohydrin and 38.9 g of potassium carbonate is stirred for 6 hours at 90°. The solids are then suction-filtered whilst hot, washed with acetonitrile and the filtrate is concentrated by evaporation in vacuo. The oil remaining crystallises when left to stand and is recrystallised from 320 ml of ethyl acetate, with carbon treatment. The resulting epoxide melts at 96°-99°.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04727067uspto-grants-1988_02