반응 #55737

ord-134ee4dc025f410bb38c262b1f0f4ea8

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere added
  2. 2
    workup.STIRRINGAfter stirring for 0.5 hour the organic phase
  3. 3
    기타was separated
  4. 4
    기타dried
  5. 5
    기타evaporated in vacuo
  6. 6
    workup.DISTILLATIONDistillation

실험 절차

Over a period of 0.5 hour 9.25 g (0.025 mol) of (3-bromopropyl) tripropyltin was added to 25 ml of 3-dimethylaminopropyl amine at room temperature. The mixture was stirred for 1 hour at 60° C. Under cooling 75 ml of diethylether and 60 ml of a 15% aqueous solution of sodium bicarbonate were added. After stirring for 0.5 hour the organic phase was separated, dried and evaporated in vacuo. Distillation gave 7.5 g (77%) of Pr3Sn(CH2)3NH(CH2)3NMe2 ; b.p. 113°-114° C./0.1 mm Hg, nD20 =1.4855.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04221811uspto-grants-1980_09