反应 #74806

ord-e2039377bfee433b9b961f74de835854

反应方程式

COc1ccc2c(c1)CCC1CCNC(=O)C(CC(C)NC(C)C)=C21
1-(2-isopropylaminopropyl)-9-methoxy-3,4,5,5a,6,7-hexahydro-2H-naphth[1,2-d]azepin-2-one
C1CO1
ethylene oxide
C1CO1
ethylene oxide
COc1ccc2c(c1)CCC1CCNC(=O)C(CC(C)N(CCO)C(C)C)=C21
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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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°.

来源

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