反応 #56202

ord-eba49821059f43c39f01dbce8588f7d9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他is placed in a 250 cm3 reaction vessel
  2. 2
    その他equipped with a stirrer
  3. 3
    workup.ADDITIONis slowly added
  4. 4
    workup.ADDITIONpoured into iced,
  5. 5
    その他A whitish oil separates and finally crystallizes
  6. 6
    その他Upon recrystallization from acetone
  7. 7
    その他a solid which melts at 106°-107° C. (capillary tube) is obtained

実験手順

6.2 g (0.084 mole+20%) of monoethanolamine dissolved in 30 cm3 of dioxane is placed in a 250 cm3 reaction vessel equipped with a stirrer, a cooler, a dropping funnel and a thermometer. At a temperature of between 15° and 20° C., a solution of 12.2 g (0.042 mole) of 5-benzoyl-indan-2-carboxylic acid chloride (prepared in conventional manner by reacting thionyl chloride with the corresponding acid) in 30 cm3 of dioxane is slowly added. The reaction mixture is stirred for one hour at ambient temperature and then poured into iced, acidified water. A whitish oil separates and finally crystallizes. Upon recrystallization from acetone, a solid which melts at 106°-107° C. (capillary tube) is obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04224341uspto-grants-1980_09