Hydrochloric Acid → HCID 178467361, compound

HRID 1418617Notes

Reaction equation

HRID 1418617 reaction equation
[CH2:1]([O:3][C:4]1[N:8]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[NH:23][O:24][C:25](=[O:27])[N:26]=3)=[CH:12][CH:11]=2)[C:7]2[C:28]([C:32]([O:34]C)=[O:33])=[CH:29][CH:30]=[CH:31][C:6]=2[N:5]=1)[CH3:2].[OH-].[Na+].Cl>CO>[CH2:1]([O:3][C:4]1[N:8]([CH2:9][C:10]2[CH:11]=[CH:12][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[NH:23][O:24][C:25](=[O:27])[N:26]=3)=[CH:14][CH:15]=2)[C:7]2[C:28]([C:32]([OH:34])=[O:33])=[CH:29][CH:30]=[CH:31][C:6]=2[N:5]=1)[CH3:2]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178418592HCID 178418592, compound

Product 1

HCID 178467361HCID 178467361, compoundYield 54.8%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
60 °C

Procedure

A mixture of the compound (0.47 g) obtained in Example (54h) and 1N NaOH (3 ml) in methanol (3 ml) was heated for 30 minutes under reflux. The reaction mixture was adjusted to pH 3-4 with 1N HCl. Resulting crystalline precipitates were collected by filtration and recrystallized from ethyl acetate-hexane. The crystals were suspended in water (2 ml), and the suspension was stirred for 2 hours at 60° C. Insoluble materials were collected by filtration and dried to afford colorless crystals (0.25 g, 54%). This product was in agreement with that obtained in Example 1.

Workup

  1. temperaturewas heated for 30 minutes
  2. temperatureunder reflux
  3. customResulting crystalline precipitates
  4. filtrationwere collected by filtration
  5. customrecrystallized from ethyl acetate-hexane
  6. filtrationInsoluble materials were collected by filtration
  7. customdried

Sources & evidence

ORD record
ord-2e1789000df047eca50ef62ecad05451
Source dataset
uspto-grants-1999_03
Patent number
US05883111

Reaction notes

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