Hydrochloric Acid → HCID 58460122, compound

HRID 709120Notes

Reaction equation

HRID 709120 reaction equation
[OH-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([NH:12][NH:13][C:14]([NH:16][CH2:17][C:18]([O:20]CC)=[O:19])=[O:15])=O)=[CH:6][CH:5]=1.Cl>>[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:16]([CH2:17][C:18]([OH:20])=[O:19])[C:14](=[O:15])[NH:13][N:12]=2)=[CH:6][CH:5]=1

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59536829HCID 59536829, compound

Product 1

HCID 58460122HCID 58460122, compound

Procedure

91 ml of a 3N aqueous sodium hydroxide solution were added to 21.43 g (67.9 mmol) of the compound of Example 1A, and the mixture was heated at reflux overnight. After cooling to RT, the mixture was adjusted to pH 1 by slow addition of about 20% strength hydrochloric acid. The precipitated solid was isolated by filtration, washed with water and dried under reduced pressure at 60° C. This gave 17.55 g of the title compound in a purity of about 88% (90% of theory).

Workup

  1. temperaturethe mixture was heated
  2. temperatureat reflux overnight
  3. customThe precipitated solid was isolated by filtration
  4. washwashed with water
  5. customdried under reduced pressure at 60° C

Sources & evidence

ORD record
ord-5f6e734295ef42ba8d1e79dd5498b726
Source dataset
uspto-grants-2015_11
Patent number
US09180120B2

Reaction notes

Loading…