Hydrochloric Acid → HCID 20267558, compound

HRID 1719125Notes

Reaction equation

HRID 1719125 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][CH2:9][CH:8]([NH:17][CH2:18][C:19]([O:21]CC)=[O:20])[C:7]1=[O:24])([OH:4])=[O:3].C(O)C.[OH-].[Na+].Cl>O>[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][CH2:9][CH:8]([NH:17][CH2:18][C:19]([OH:21])=[O:20])[C:7]1=[O:24])([OH:4])=[O:3]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 13454590HCID 13454590, compound

Product 1

HCID 20267558HCID 20267558, compoundYield 90.1%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

420 mg of the 5-carboxymethyl-3-ethoxycarbonylmethylamino-2,3-dihydro-1,5-benzothiazepin-4(5H)-one hydrochloride obtained in Example 15 was dissolved in 5 ml of water, 3 ml of ethanol and 3.5 ml of a 1N aqueous solution of sodium hydroxide and then reacted for 2 hours. Thereafter, the solution was adjusted to pH 1-2 with hydrochloric acid and concentrated to dryness under reduced pressure. Ethanol was added to the residue and the insoluble matter was filtered off. After the filtrate was concentrated, ether was added thereto so as to cause crystallization. Thus, there was obtained 350 mg of the desired compound.

Workup

  1. concentrationconcentrated to dryness under reduced pressure
  2. additionEthanol was added to the residue
  3. filtrationthe insoluble matter was filtered off
  4. concentrationAfter the filtrate was concentrated
  5. additionether was added
  6. customcrystallization

Sources & evidence

ORD record
ord-288ae281fe3f4be49630f46ec3535a7e
Source dataset
uspto-grants-1985_09
Patent number
US04539150

Reaction notes

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