Water → 1-[1-(4-Chlorophenyl)cyclobutyl]-N,N,3-trimethylbutan-1-amine--hydrogen chloride--water (1/1/1)

HRID 974529Notes

Reaction equation

HRID 974529 reaction equation
Cl.[CH3:2][N:3]([CH:5]([C:10]1([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[CH2:13][CH2:12][CH2:11]1)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:4].[OH2:21]>>[OH2:21].[ClH:20].[CH3:2][N:3]([CH:5]([C:10]1([C:14]2[CH:15]=[CH:16][C:17]([Cl:20])=[CH:18][CH:19]=2)[CH2:13][CH2:12][CH2:11]1)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:4]

Participants

3

Reactant 2

HCID 962WaterHCID 64764Sibutramine hydrochloride

Product 1

HCID 647651-[1-(4-Chlorophenyl)cyclobutyl]-N,N,3-trimethylbutan-1-amine--hydrogen chloride--water (1/1/1)

Procedure

A sample (1 g) of N,N-dimethyl-1-[1-(4-chlorophenyl)cyclobutyl]-3-methylbutylamine hydrochloride which had been dehydrated in vacuo at 70° C. for 7 hours was dissolved in a boiling mixture of water (0.5 ml) and an organic solvent (4.5 ml). The solution was allowed to cool to ambient temperature and then stored at 4° C. for three hours. A solid was collected by filtration, washed with the organic solvent and dried in vacuo at ambient temperature for 18 hours to give N,N-dimethyl-1-[1-(4-chlorophenyl)cyclobutyl]-3-methylbutylamine hydrochloride monohydrate the melting point of which is given below.

Workup

  1. filtrationA solid was collected by filtration
  2. washwashed with the organic solvent
  3. customdried in vacuo at ambient temperature for 18 hours

Sources & evidence

ORD record
ord-9de75bd130cd45eda8d7a7840f5de423
Source dataset
uspto-grants-1991_11
Patent number
US05068440

Reaction notes

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