반응 #74797

ord-c75ca27004304944a8afb4a0dfc8fbcd

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the organic layer is separated
  2. 2
    세척washed with water
  3. 3
    기타dried
  4. 4
    기타evaporated
  5. 5
    기타The residue is crystallized from diethyl ether
  6. 6
    기타recrystallized from ethyl acetate

실험 절차

To the stirred suspension of 4 g of 1-chloromethyl-3,4,5,5a,6,7-hexahydro-9-methoxy-2H-naphth[1,2-d]azepin-2-one in 80 ml of methylene chloride is added 8 ml of isopropylamine. The mixture is stirred at room temperature overnight, 80 ml of saturated aqueous sodium carbonate are added, the organic layer is separated, washed with water, dried and evaporated. The residue is crystallized from diethyl ether and recrystallized from ethyl acetate, to give the 1-isopropylaminomethyl-3,4,5,5a, 6,7-hexahydro-9-methoxy-2H-naphth[1,2-d]azepin-2-one melting at 212°-214°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04173633uspto-grants-1979_11