Hydrochloric Acid → HCID 70143924, compound

HRID 381285Notes

Reaction equation

HRID 381285 reaction equation
[OH-].[Na+].[CH:3]1([C:9]2[O:14][C:13]3[C:15]([C:18]([O:20]C)=[O:19])=[CH:16][S:17][C:12]=3[C:11](=[O:22])[CH:10]=2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.Cl>CO.O1CCOCC1.O>[CH:3]1([C:9]2([C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=3)[O:14][C:13]3[C:15]([C:18]([OH:20])=[O:19])=[CH:16][S:17][C:12]=3[C:11](=[O:22])[CH2:10]2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1

Participants

7

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 18399621HCID 18399621, compound

Product 1

HCID 70143924HCID 70143924, compoundYield 114.8%

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 962WaterSolvent2×HCID 312751,4-DioxaneSolvent

Conditions

Temperature
50 °C

Procedure

0.3 mL of 1N sodium hydroxide and 1.0 mL of water were added to a solution of 0.040 g of Compound 3D in 1.8 mL of MeOH and 0.9 mL of 1,4-dioxane at 20-25° C., while stirring. The mixture was heated at 50° C. for 3.5 hours. After cooling to 20-25° C., the mixture was diluted with water and acidified to pH 1 with 3N hydrochloric acid. The precipitated solid was collected by filtration and washed with water to afford 0.028 g (73.5%) of the title compound, melting at 269-275° C.

Workup

  1. temperatureAfter cooling to 20-25° C.
  2. filtrationThe precipitated solid was collected by filtration
  3. washwashed with water

Sources & evidence

ORD record
ord-a246eae0c8e94d08bd24a6d30afef420
Source dataset
uspto-grants-2001_10
Patent number
US06306861B1

Reaction notes

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