Hydrochloric Acid → HCID 178423663, compound

HRID 1169416Notes

Reaction equation

HRID 1169416 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH2:16][C@H:17]2[CH2:22][CH2:21][C@H:20]([NH:23][C:24]([C:26]3[CH2:27][CH2:28][O:29][C:30]4[CH:36]=[CH:35][C:34]([C:37]5[CH:42]=[CH:41][C:40]([CH3:43])=[CH:39][CH:38]=5)=[CH:33][C:31]=4[CH:32]=3)=[O:25])[CH2:19][CH2:18]2)[CH3:15])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:44]>C(O)C>[ClH:44].[ClH:44].[NH:8]1[CH2:9][CH2:10][CH:11]([N:14]([CH2:16][C@H:17]2[CH2:18][CH2:19][C@H:20]([NH:23][C:24]([C:26]3[CH2:27][CH2:28][O:29][C:30]4[CH:36]=[CH:35][C:34]([C:37]5[CH:38]=[CH:39][C:40]([CH3:43])=[CH:41][CH:42]=5)=[CH:33][C:31]=4[CH:32]=3)=[O:25])[CH2:21][CH2:22]2)[CH3:15])[CH2:12][CH2:13]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 178423664HCID 178423664, compound

Product 1

HCID 178423663HCID 178423663, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Into a solution of trans-N-[4-[N-(1-tert-butoxycarbonylpiperidin-4-yl)-N-methylaminomethyl]cyclohexyl]-7-(4-methylphenyl)-2,3-dihydro-1-benzooxepine-4-carboxamide (0.41 g) in ethanol (30 ml) was added at room temperature concentrated hydrochloric acid (5 ml), and the resulting mixture was stirred for 2 days. After the reaction mixture was concentrated under reduced pressure, the resulting crystals were purified by recrystallization (ethanol/diethyl ether) to obtain trans-N-[4-[N-(piperidin-4-yl)-N-methylaminomethyl]cyclohexyl]-7-(4-methylphenyl)-2,3-dihydro-1-benzooxepine-4-carboxamide dihydrochloride (compound 66) (381 mg) as colorless crystals.

Workup

  1. concentrationAfter the reaction mixture was concentrated under reduced pressure
  2. customthe resulting crystals were purified by recrystallization (ethanol/diethyl ether)

Sources & evidence

ORD record
ord-a2ebd50b3e784e96801470f9a3a83b69
Source dataset
uspto-grants-2003_09
Patent number
US06627651B1

Reaction notes

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