Hydrochloric Acid → HCID 178457597, compound

HRID 1266908Notes

Reaction equation

HRID 1266908 reaction equation
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]([O:6][CH2:7][CH2:8][CH2:9][O:10][NH:11][C:12]([NH:14][C:15]([NH:17][CH:18]([CH3:20])[CH3:19])=[NH:16])=[NH:13])=[CH:4][CH:3]=1.[ClH:23]>CCOC(C)=O>[ClH:1].[ClH:23].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH2:7][CH2:8][CH2:9][O:10][NH:11][C:12]([NH:14][C:15]([NH:17][CH:18]([CH3:19])[CH3:20])=[NH:16])=[NH:13])=[CH:21][CH:22]=1

Participants

4

Reactant 2

HCID 313Hydrochloric Acid2×HCID 178457595HCID 178457595, compound

Product 1

HCID 178457597HCID 178457597, compoundYield 99%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent4×

Procedure

A mixture of 656 g (2.00 mole) of 1-[3(4-Chlorophenoxy)propyloxy-5-isopropylbiguanide and 1.0 L of EtOAc was swirled and cooled in an ice bath before 500 g of EtOAc containing 74.5 (2.04 moles) of HCl was added. After 10 minutes a second 500 g (2.04 moles) of the HCl in EtOAc was added in small portions with swirling and cooling in the ice bath. The thick precipitate was thinned with 500 mL of EtOAc. After air-drying the material was ground with a mortar and pestle, dried at 50° C., and then at a vacuum of 1 mm to give 793 g (99%) of product mp 160-165° C.

Workup

  1. additionwas added
  2. customAfter air-drying the material
  3. customdried at 50° C.

Sources & evidence

ORD record
ord-8f1f4bc24e2245339cb5d1380f2bb486
Source dataset
uspto-grants-2003_04
Patent number
US06551614B2

Reaction notes

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