Hydrochloric Acid → HCID 178437445, compound

HRID 1707718Notes

Reaction equation

HRID 1707718 reaction equation
[CH2:1]([C:3]1[N:16]([CH2:17][C:18]2[CH:23]=[CH:22][C:21]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:30]3[NH:31][O:32][C:33](=[O:35])[N:34]=3)=[CH:20][CH:19]=2)[C:6]2=[N:7][C:8]([C:12]([O:14]C)=[O:13])=[CH:9][C:10]([CH3:11])=[C:5]2[N:4]=1)[CH3:2].[OH-].[Na+].Cl>CO>[CH2:1]([C:3]1[N:16]([CH2:17][C:18]2[CH:19]=[CH:20][C:21]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[C:30]3[NH:31][O:32][C:33](=[O:35])[N:34]=3)=[CH:22][CH:23]=2)[C:6]2=[N:7][C:8]([C:12]([OH:14])=[O:13])=[CH:9][C:10]([CH3:11])=[C:5]2[N:4]=1)[CH3:2]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178437444HCID 178437444, compound

Product 1

HCID 178437445HCID 178437445, compoundYield 69.9%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
60 °C

Procedure

To a suspension of the compound (0.9 g) obtained in Example (56g) in methanol (20 ml) was added 1N aqueous solution of sodium hydroxide (4.5 ml), and the mixture was stirred for 3 hours at 60° C. To the reaction mixture was added 1N HCl to adjust the pH to 3-4. Resulting crystalline precipitates were collected by filtration and dried. Crude crystals thus obtained were recrystallized from ethyl acetate--methanol afforded the title compound as colorless crystals (0.61 g, 69%), m.p.261°-164° C. (decomp.).

Workup

  1. customResulting crystalline precipitates
  2. filtrationwere collected by filtration
  3. customdried
  4. customCrude crystals thus obtained
  5. customwere recrystallized from ethyl acetate

Sources & evidence

ORD record
ord-b2c1940f666e4e1ca7644de384129e24
Source dataset
uspto-grants-1994_10
Patent number
US05354766

Reaction notes

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