反应 #521787

ord-e99a89b33de040799c68d0da75ab09d9

反应方程式

CCC1(CCC(=O)O)CCC[N+]2=C1c1[nH]c3ccccc3c1CC2C(=O)O.[O-][Cl+3]([O-])([O-])[O-]
(+)-1α-ethyl-1β- carboxyethyl-6-carboxy-1,2,3,4,6,7-hexahydro-12H-indolo(2,3-a)-quinolizin-5-ium perchlorate
C1CCC2CCCCC2C1
decalin
CCC1(CCC(=O)O)CCC[N+]2=C1c1[nH]c3ccccc3c1CC2.[O-][Cl+3]([O-])([O-])[O-]
title compound
收率 97.2%
CCC1(CCC(=O)O)CCC[N+]2=C1c1[nH]c3ccccc3c1CC2.[O-][Cl+3]([O-])([O-])[O-]
(-)-1α-Ethyl-1β- carboxyethyl-1,2,3,4,6,7-hexahydro-12H-indolo(2,3-a)quinolizin-5-ium perchlorate
收率 97.2%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling the reaction mixture
  2. 2
    过滤is filtered
  3. 3
    其他the solid obtained
  4. 4
    洗涤is washed decalin-free with three 5-ml
  5. 5
    干燥portions of ether and is dried

实验过程

1000 mg. (2.13 mmoles) of (+)-1α-ethyl-1β- carboxyethyl-6-carboxy-1,2,3,4,6,7-hexahydro-12H-indolo(2,3-a)-quinolizin-5-ium perchlorate in 15 ml. of decalin are heated at 160° to 170° C. for 25 minutes, with stirring. The substance melts accompanied by gas evolution. After cooling the reaction mixture is filtered, the solid obtained is washed decalin-free with three 5-ml. portions of ether and is dried. 880 mg. of the title compound are obtained. Yield: 97.2% [α]D25 =-19°.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04399069uspto-grants-1983_08