Hydrochloric Acid → Ivabradine Hydrochloride

HRID 625924Notes

Reaction equation

HRID 625924 reaction equation
[CH3:1][N:2]([CH2:22][C@@H:23]1[C:26]2[CH:27]=[C:28]([O:33][CH3:34])[C:29]([O:31][CH3:32])=[CH:30][C:25]=2[CH2:24]1)[CH2:3][CH2:4][CH2:5][N:6]1[C:16](=[O:17])[CH2:15][C:14]2[C:9](=[CH:10][C:11]([O:20][CH3:21])=[C:12]([O:18][CH3:19])[CH:13]=2)[CH2:8][CH2:7]1.[ClH:35]>C1(C)C=CC=CC=1.C(O)C>[CH3:1][N:2]([CH2:22][C@@H:23]1[C:26]2[CH:27]=[C:28]([O:33][CH3:34])[C:29]([O:31][CH3:32])=[CH:30][C:25]=2[CH2:24]1)[CH2:3][CH2:4][CH2:5][N:6]1[C:16](=[O:17])[CH2:15][C:14]2[C:9](=[CH:10][C:11]([O:20][CH3:21])=[C:12]([O:18][CH3:19])[CH:13]=2)[CH2:8][CH2:7]1.[ClH:35]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 132999Ivabradine

Product 1

HCID 3045381Ivabradine Hydrochloride

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 1140TolueneSolvent

Procedure

A solution which comprised 6.9 g of ivabradine in 90 mL of toluene was stirred maintaining the temperature below about 40° C. 16 ml of a chlorhydric acid solution in ethanol 1.75M were added. The solution was seeded with the product obtained in the Example 1. Crystal growth was promoted by stirring for 20 hours maintaining the temperature below about 40° C. The solid product obtained was isolated and dried under vacuum at a temperature of 65° C.

Workup

  1. temperaturemaintaining the temperature below about 40° C
  2. customobtained in the Example 1
  3. stirringby stirring for 20 hours
  4. temperaturemaintaining the temperature below about 40° C
  5. customThe solid product obtained
  6. customwas isolated
  7. customdried under vacuum at a temperature of 65° C.

Sources & evidence

ORD record
ord-1f441aff29c5494ba9cc9e7cb83f7577
Source dataset
uspto-grants-2016_04
Patent number
US09309201B2

Reaction notes

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