Hydrochloric Acid → HCID 68488327, compound

HRID 389025Notes

Reaction equation

HRID 389025 reaction equation
Cl.C(O)C.C([O:7][C:8](=[O:34])[CH2:9][C:10]1[S:11][C:12]2[C:13]([O:32]C)=[CH:14][C:15]3[CH:31]=[CH:30][CH:29]=[CH:28][C:16]=3[C:17](O)([CH:20]3[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]3)[C:18]=2[CH:19]=1)C.[OH-].[Na+]>O>[CH3:26][N:23]1[CH2:22][CH2:21][C:20](=[C:17]2[C:16]3[CH:28]=[CH:29][CH:30]=[CH:31][C:15]=3[CH2:14][C:13](=[O:32])[C:12]3[S:11][C:10]([CH2:9][C:8]([OH:34])=[O:7])=[CH:19][C:18]2=3)[CH2:25][CH2:24]1

Participants

6

Reactant 4

HCID 313Hydrochloric Acid2×HCID 702EthanolHCID 14798Sodium HydroxideHCID 86649441HCID 86649441, compound

Product 1

HCID 68488327HCID 68488327, compoundYield 39.4%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Hydrochloric acid (8 mL) was added to an ethanol (24 mL) solution of the compound obtained in Example 16 (2.0 g, 4.7 mmol), and the mixture was refluxed while heating overnight. The solvents were distilled off, water (20 mL) and sodium hydroxide (0.8 g, 20 mmol) were then added to the residue, and the mixture was stirred at room temperature overnight. The property of the solution is adjusted to a pH of 6.5 with hydrochloric acid, and the precipitated crystals were separated by filtration and dried, to give 0.68 g (39%) of the captioned compound.

Workup

  1. temperaturethe mixture was refluxed
  2. temperaturewhile heating overnight
  3. distillationThe solvents were distilled off
  4. customthe precipitated crystals were separated by filtration
  5. customdried

Sources & evidence

ORD record
ord-41cde8b2c7214052878b26985a13754e
Source dataset
uspto-grants-2013_02
Patent number
US08377967B2

Reaction notes

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