Hydrochloric Acid → HCID 178467361, compound

HRID 1080828Notes

Reaction equation

HRID 1080828 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>>[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

4

Reactant 3

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

Product 1

HCID 178467361HCID 178467361, compoundYield 54.8%

Conditions

Temperature
60 °C

Procedure

A mixture of the compound (0.47 g) obtained in Example (54h) and 1N NaOH (3 ml) in methan61 (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
  6. filtrationInsoluble materials were collected by filtration
  7. customdried

Sources & evidence

ORD record
ord-59c02638e9524968be1944ddba3e4de1
Source dataset
uspto-grants-1996_12
Patent number
US05583141

Reaction notes

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