Hydrochloric Acid → HCID 72714301, compound

HRID 1453536Notes

Reaction equation

HRID 1453536 reaction equation
[Cl:1][C:2]1[S:10][C:9]2[S:8](=[O:12])(=[O:11])[N:7]=[CH:6][N:5]([CH2:13][CH2:14][F:15])[C:4]=2[CH:3]=1.[BH4-].[Na+].Cl>C(O)(C)C.O>[Cl:1][C:2]1[S:10][C:9]2[S:8](=[O:12])(=[O:11])[NH:7][CH2:6][N:5]([CH2:13][CH2:14][F:15])[C:4]=2[CH:3]=1

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 72714296HCID 72714296, compound

Product 1

HCID 72714301HCID 72714301, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 3776IsopropanolSolvent

Conditions

Temperature
60 °C

Procedure

100 mg of the compound obtained in Step A above are dissolved in 4 ml of isopropanol. The mixture is heated to 60° C., then 200 mg of sodium borohydride are added. After minutes at that temperature, the solvent is evaporated off under reduced pressure. The residue that is obtained is taken up in 10 ml of water, cooled in an ice bath and adjusted to pH 4 by addition of 6N hydrochloric acid. The insoluble material is collected by filtration and washed with water. The product is then dissolved in a minimum of chloroform and precipitated by addition of n-hexane. The precipitate is then collected by filtration.

Workup

  1. waitAfter minutes at that temperature
  2. customthe solvent is evaporated off under reduced pressure
  3. customThe residue that is obtained
  4. temperaturecooled in an ice bath
  5. filtrationThe insoluble material is collected by filtration
  6. washwashed with water
  7. dissolutionThe product is then dissolved in a minimum of chloroform
  8. customprecipitated by addition of n-hexane
  9. filtrationThe precipitate is then collected by filtration

Sources & evidence

ORD record
ord-fe51b3a1e3e84130921f8b1ed4bada14
Source dataset
uspto-grants-2009_01
Patent number
US07476668B2

Reaction notes

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