Hydrochloric Acid → HCID 25258036, compound

HRID 2265108Notes

Reaction equation

HRID 2265108 reaction equation
[CH3:1][Si:2]([CH3:32])([CH3:31])[C:3]1[CH:4]=[C:5]([CH:24]=[C:25]([Si:27]([CH3:30])([CH3:29])[CH3:28])[CH:26]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12](/[CH:15]=[C:16](\[CH3:22])/[C:17]([O:19]CC)=[O:18])=[C:11]([F:23])[CH:10]=1)=[O:7].[OH-].[Na+].Cl>C(O)C>[CH3:30][Si:27]([CH3:28])([CH3:29])[C:25]1[CH:24]=[C:5]([CH:4]=[C:3]([Si:2]([CH3:1])([CH3:32])[CH3:31])[CH:26]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12](/[CH:15]=[C:16](\[CH3:22])/[C:17]([OH:19])=[O:18])=[C:11]([F:23])[CH:10]=1)=[O:7]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86644286HCID 86644286, compound

Product 1

HCID 25258036HCID 25258036, compoundYield 86%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
50 °C

Procedure

Compound 14e (18.9 g) was dissolved in ethanol (302 ml), and a 2N sodium hydroxide aqueous solution (100 ml) was added thereto. The obtained mixture was stirred under heating at 50° C. for 2 hours. The reaction mixture was ice-cooled, and a 1N hydrochloric acid aqueous solution (300 ml) was added to neutralize the mixture. The precipitated solid was filtered off and dried under reduced pressure to obtain Crude Compound 14 (16.6 g) as a white solid. Crude Compound 14 (400 mg) was recrystallized with ethanol (4.0 ml) and purified water (4.0 ml) to obtain Compound 14 (344 mg, 86%) as a white solid.

Workup

  1. temperaturecooled
  2. filtrationThe precipitated solid was filtered off
  3. customdried under reduced pressure
  4. customto obtain Crude Compound 14 (16.6 g) as a white solid
  5. customCrude Compound 14 (400 mg) was recrystallized with ethanol (4.0 ml)
  6. custompurified water (4.0 ml)

Sources & evidence

ORD record
ord-1b1377afc4c14841a3022b4c97c27f2f
Source dataset
uspto-grants-2010_12
Patent number
US07855300B2

Reaction notes

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