Hydrochloric Acid → HCID 19868623, compound

HRID 330488Notes

Reaction equation

HRID 330488 reaction equation
[NH2:1][CH2:2][C:3]([O:5][C:6]1[CH:21]=[C:20]([O:22][C:23](=[O:26])[CH2:24][NH2:25])[C:9]2[C:10]([CH3:19])=[C:11]3[N:16]([C:17](=[O:18])[C:8]=2[CH:7]=1)[CH2:15][CH2:14][CH2:13][CH2:12]3)=[O:4].[ClH:27]>ClCCl>[ClH:27].[ClH:27].[NH2:1][CH2:2][C:3]([O:5][C:6]1[CH:21]=[C:20]([O:22][C:23](=[O:26])[CH2:24][NH2:25])[C:9]2[C:10]([CH3:19])=[C:11]3[N:16]([C:17](=[O:18])[C:8]=2[CH:7]=1)[CH2:15][CH2:14][CH2:13][CH2:12]3)=[O:4]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 19868624HCID 19868624, compound

Product 1

HCID 19868623HCID 19868623, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
25 °C

Procedure

Dissolve 8,10-bis[(aminoacetyl)oxy]-11-methyl-1,2,3,4-tetrahydro-6H-benzo[b]quinolizine-6-one (0.92 g) in dry dichloromethane (100 ml), and pass a stream of hydrogen chloride gas through the solution for 45 min. at ambient temperature (about 25° C.). Stir the resulting mixture at 25° C. for 2 hours, and filter to collect the precipitated crystals. Wash the collected crystals with ether and acetone, and dry and crystallize them to obtain 8,10-bis[(aminoacetyl)oxy]-11-methyl-1,2,3,4-tetrahydro-6H-benzo[b]quinolizine-6-one dihydrochloride, m.p. 202°-205° C. (from MeOH-ether, as a hemihydrate).

Workup

  1. customfor 45 min.
  2. customat ambient temperature
  3. custom(about 25° C.)
  4. filtrationfilter
  5. customto collect the precipitated crystals
  6. washWash the collected crystals with ether and acetone
  7. customdry
  8. customcrystallize them

Sources & evidence

ORD record
ord-8058d5f4771542daa67bb96556babb30
Source dataset
uspto-grants-1990_01
Patent number
US04897391

Reaction notes

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