Hydrochloric Acid → HCID 54065715, compound

HRID 1762690Notes

Reaction equation

HRID 1762690 reaction equation
[OH-].[Na+].C([O:5][C:6]([C:8]1[NH:9][N:10]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[S:21]([OH:24])(=[O:23])=[O:22])[C:11](=[O:13])[CH:12]=1)=[O:7])C.Cl>O>[C:6]([C:8]1[NH:9][N:10]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[S:21]([OH:24])(=[O:22])=[O:23])[C:11](=[O:13])[CH:12]=1)([OH:7])=[O:5]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 53910740HCID 53910740, compound

Product 1

HCID 54065715HCID 54065715, compoundYield 87%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
70 °C

Procedure

To a solution prepared by dissolving 7.8 g of sodium hydroxide in 20 ml of water was added 17.9 g of Intermediate A, and the resulting mixture was heated with stirring for 5 hours at a reaction mixture temperature of 70° C. After cooling the reaction mixture to room temperature, 16 ml of concentrated hydrochloric acid was added thereto, and the concentration treatment was continued under reduced pressure until a white crystalline precipitate started to separate from the reaction mixture, and then the concentrated solution was cooled with ice-cold water to precipitate the white crystals. These crystals were filtered off, washed with acetone, and dried. Thus, 14.2 g (yield: 87%) of Intermediate B was obtained. Melting Point: 223°-226° C.

Workup

  1. customTo a solution prepared
  2. temperaturethe resulting mixture was heated
  3. temperatureAfter cooling the reaction mixture to room temperature
  4. customto separate from the reaction mixture
  5. temperaturethe concentrated solution was cooled with ice-cold water
  6. customto precipitate the white crystals
  7. filtrationThese crystals were filtered off
  8. washwashed with acetone
  9. customdried

Sources & evidence

ORD record
ord-1f674a82c9374c30a8cf42835f3d5383
Source dataset
uspto-grants-1989_05
Patent number
US04833246

Reaction notes

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