Hydrochloric Acid → HCID 53892030, compound

HRID 442857Notes

Reaction equation

HRID 442857 reaction equation
[CH3:1][N:2]([CH3:43])[CH2:3][CH2:4][NH:5][C:6]([C:8]1[N:9]([CH2:38][CH2:39][N:40]([CH3:42])[CH3:41])[C:10]2[C:15]([C:16]=1[CH:17]([C:28]1[CH:33]=[CH:32][C:31]([O:34]COC)=[CH:30][CH:29]=1)[C:18]1[CH:23]=[CH:22][C:21]([O:24]COC)=[CH:20][CH:19]=1)=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:7].Cl.C(=O)(O)[O-].[Na+].C(OCC)(=O)C>C(O)C>[CH3:43][N:2]([CH3:1])[CH2:3][CH2:4][NH:5][C:6]([C:8]1[N:9]([CH2:38][CH2:39][N:40]([CH3:42])[CH3:41])[C:10]2[C:15]([C:16]=1[CH:17]([C:28]1[CH:33]=[CH:32][C:31]([OH:34])=[CH:30][CH:29]=1)[C:18]1[CH:23]=[CH:22][C:21]([OH:24])=[CH:20][CH:19]=1)=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:7]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 67594251HCID 67594251, compound

Product 1

HCID 53892030HCID 53892030, compoundYield 81%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Compound 49 (2.48 g, 4.21 mmol) obtained in Example 49 was dissolved in ethanol (50 ml), and 15 ml of 2N hydrochloric acid was added thereto, followed by heating under reflux for 2 hours. After cooling the reaction solution, a saturated aqueous solution of sodium bicarbonate was added thereto for neutralization. A little amount of ethyl acetate was added to the mixture followed by stirring at room temperature. The resulting crystals were collected by filtration, washed with water, and dried under reduced pressure to give 1.6 g (yield: 81%) of the title compound.

Workup

  1. temperatureby heating
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling the reaction solution
  4. filtrationThe resulting crystals were collected by filtration
  5. washwashed with water
  6. customdried under reduced pressure

Sources & evidence

ORD record
ord-c04067ad5f144e0a8195389a95124cc0
Source dataset
uspto-grants-1999_04
Patent number
US05891902

Reaction notes

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