반응 #56202

ord-eba49821059f43c39f01dbce8588f7d9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04224341uspto-grants-1980_09