HCID 20313708, compound → HCID 20313656, compound

HRID 2419592Notes

Reaction equation

HRID 2419592 reaction equation
[OH2:1].O.O.[ClH:4].Cl.Cl.[CH3:7][O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][C:18]=1[O:19][CH3:20])[CH:15]([CH2:21][CH2:22][CH:23]([CH2:40][CH2:41][CH2:42][CH2:43][CH:44]1[C:53]3[C:48](=[CH:49][C:50]([O:56][CH3:57])=[C:51]([O:54][CH3:55])[CH:52]=3)[CH2:47][CH2:46][NH:45]1)[CH2:24][CH2:25][CH:26]1[C:35]3[C:30](=[CH:31][C:32]([O:38][CH3:39])=[C:33]([O:36][CH3:37])[CH:34]=3)[CH2:29][CH2:28][NH:27]1)[NH:14][CH2:13][CH2:12]2>CCOCC.C(Cl)(Cl)Cl>[OH2:8].[OH2:1].[OH2:8].[ClH:4].[ClH:4].[ClH:4].[CH3:7][O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][C:18]=1[O:19][CH3:20])[C:15]([CH2:21][CH2:22][CH:23]([CH2:40][CH2:41][CH2:42][CH2:43][C:44]1[C:53]3[C:48](=[CH:49][C:50]([O:56][CH3:57])=[C:51]([O:54][CH3:55])[CH:52]=3)[CH2:47][CH2:46][N:45]=1)[CH2:24][CH2:25][C:26]1[C:35]3[C:30](=[CH:31][C:32]([O:38][CH3:39])=[C:33]([O:36][CH3:37])[CH:34]=3)[CH2:29][CH2:28][N:27]=1)=[N:14][CH2:13][CH2:12]2

Participants

4

Reactant 1

HCID 20313708HCID 20313708, compound

Product 1

HCID 20313656HCID 20313656, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 6212ChloroformSolvent2×

Procedure

To purify the intermediate (1.1a), the crude residue obtained after stripping off the chloroform is converted to the hydrochloride, in ether, and the resulting salt taken up in chloroform. Precipitation with ether, followed by two further reprecipitations from chloroform solution by either yields (1.1a) 1,1'-{3-[2-(3,4-dihydro-6,7-dimethoxy-1-isoquinolinyl)ethyl]heptamethylene}bis[3,4-dihydro-6,7-dimethoxyisoquinoline] trihydrochloride trihydrate, as a yellow solid, m.p. 130-150° (dec.).

Workup

  1. customTo purify the intermediate (1.1a)
  2. customthe crude residue obtained
  3. customPrecipitation with ether
  4. customfollowed by two further reprecipitations from chloroform solution by

Sources & evidence

ORD record
ord-c4cc6f89b116429981af74f7ea61abc0
Source dataset
uspto-grants-1978_08
Patent number
US04107165

Reaction notes

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