Perchloric Acid → HCID 13233239, compound

HRID 1263270Notes

Reaction equation

HRID 1263270 reaction equation
C[O-].[CH2:3]([C:5]1([CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26])[C:14]2[C:13]3[NH:15][C:16]4[C:21]([C:12]=3[CH2:11][CH2:10][N+:9]=2[CH2:8][CH2:7][CH2:6]1)=[CH:20][C:19]([Br:22])=[CH:18][CH:17]=4)[CH3:4].[Cl:29]([OH:33])(=[O:32])(=[O:31])=[O:30]>CO>[Cl:29]([O-:33])(=[O:32])(=[O:31])=[O:30].[CH2:3]([C:5]1([CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26])[C:14]2[C:13]3[NH:15][C:16]4[C:21]([C:12]=3[CH2:11][CH2:10][N+:9]=2[CH2:8][CH2:7][CH2:6]1)=[CH:20][C:19]([Br:22])=[CH:18][CH:17]=4)[CH3:4]

Participants

4

Reactant 2

HCID 24247Perchloric AcidHCID 20455130HCID 20455130, compound

Product 1

HCID 13233239HCID 13233239, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

0.1 g. of 1-ethyl-1-(2'-methoxycarbonylethyl)-9-bromo-1,2,3,4,6,7-hexahydro-12H-indolo[2,3-a]quinolizin-5-ium methoxide (prepared as described in Example 7) are suspended in 1 ml. of methanol, and the pH of the suspension is adjusted to 6 by introducing a 70% aqueous perchloric acid solution. The separated crystalline product is filtered off, washed with a small amount of methanol and dried. In this way 0.095 g. of 1-ethyl-1-(2'-methoxycarbonylethyl)-9-bromo-1,2,3,4,6,7-hexahydro-12H-indolo[2,3-a]quinolizin-5-ium perchlorate are obtained; m.p.: 221°-222° C. (after recrystallization from methanol).

Workup

  1. filtrationThe separated crystalline product is filtered off
  2. washwashed with a small amount of methanol
  3. customdried

Sources & evidence

ORD record
ord-110313f0f0964ceeae92ed780c4b487a
Source dataset
uspto-grants-1984_06
Patent number
US04456607

Reaction notes

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