反応 #981284

ord-571992d467c5472482e41e089b4a2d10

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他at 25° to 30° C
  2. 2
    workup.ADDITIONOn complete addition the mixture
  3. 3
    workup.STIRRINGthe mixture was stirred for 15 minutes
  4. 4
    ろ過The precipitate was filtered off
  5. 5
    洗浄washed with water and ice-cold ethanol
  6. 6
    その他dried at 60° C. in vacuo

実験手順

A solution of p-glycidyloxybenzaldehyde (40 g; prepared according to Method A) and cyclopentanone (9.4 g) in ethanol (40 g) was added over 1 hour to a stirred solution of sodium hydroxide (2.25 g) in a mixture of water (45 g) and ethanol (40 g), keeping the temperature at 25° to 30° C. On complete addition the mixture was stirred at 25° to 30° C. for a further 30 minutes, then water (100 g) was added and the mixture was stirred for 15 minutes. The precipitate was filtered off, washed with water and ice-cold ethanol, and dried at 60° C. in vacuo to give 1,3-bis(p-glycidyloxyphenylmethylidene)cyclopentan-2-one. The yield was 40 g (88% of theory) and the product had an epoxide content of 4.43 equivalents per kilogram, the theoretical value being 4.95 equivalents per kilogram. The N.M.R., I.R., and UV spectra of the product were consistent with the above structure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04282353uspto-grants-1981_08