Hydrochloric Acid → HCID 13536032, compound

HRID 1719133Notes

Reaction equation

HRID 1719133 reaction equation
[ClH:1].[C:2]([CH2:5][N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[S:10][CH:9]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:8]([NH:23][CH2:24][C:25]([O:27]CC)=[O:26])[C:7]1=[O:30])([OH:4])=[O:3].[OH-].[Na+].Cl>C(O)C>[ClH:1].[C:2]([CH2:5][N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[S:10][CH:9]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:8]([NH:23][CH2:24][C:25]([OH:27])=[O:26])[C:7]1=[O:30])([OH:4])=[O:3]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 13533194HCID 13533194, compound

Product 1

HCID 13536032HCID 13536032, compoundYield 85.8%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

410 mg of the compound obtained in Example 25 was dissolved in a mixture consisting of 3.5 ml of a 1N aqueous solution of sodium hydroxide and 5 ml of ethanol, and the resulting solution was stirred for 30 minutes. Then, the solution was adjusted to pH 1-2 with concentrated hydrochloric acid and concentrated to dryness under reduced pressure. The residue was dissolved in ethanol and the insoluble matter was filtered off. After the filtrate was concentrated, ether was added thereto so as to cause crystallization. The precipitated crystals were separated by filtration and washed with ether to obtain 330 mg of the desired compound.

Workup

  1. concentrationconcentrated to dryness under reduced pressure
  2. dissolutionThe residue was dissolved in ethanol
  3. filtrationthe insoluble matter was filtered off
  4. concentrationAfter the filtrate was concentrated
  5. additionether was added
  6. customcrystallization
  7. customThe precipitated crystals were separated by filtration
  8. washwashed with ether

Sources & evidence

ORD record
ord-4f67ed02668c4d9e9710ce75eb7f0fde
Source dataset
uspto-grants-1985_09
Patent number
US04539150

Reaction notes

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