反応 #74806

ord-e2039377bfee433b9b961f74de835854

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThe mixture of 5 g
  2. 2
    workup.STIRRINGstirred for four additional days at room temperature
  3. 3
    その他It is evaporated
  4. 4
    ろ過collected by filtration
  5. 5
    その他recrystallized from ethyl acetate

実験手順

The mixture of 5 g of slow moving 1-(2-isopropylaminopropyl)-9-methoxy-3,4,5,5a,6,7-hexahydro-2H-naphth[1,2-d]azepin-2-one and 14.75 ml of liquified ethylene oxide in 100 ml of absolute ethanol is stirred in a sealed pressure tube at room temperature for two days. The reaction mixture is recharged with an additional 14.75 ml portion of ethylene oxide and stirred for four additional days at room temperature. It is evaporated, the residue slurried in diethyl ether, collected by filtration and recrystallized from ethyl acetate to yield the 1-[2-(N-isopropyl-N-2-hydroxyethylamino)-propyl]-9-methoxy-3,4,5,5a,6,7-hexahydro-2H-naphth[1,2-d]azepin-2-one, RR racemate melting at 147°-149°.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04173633uspto-grants-1979_11