Hydrochloric Acid → HCID 11977100, compound

HRID 572143Notes

Reaction equation

HRID 572143 reaction equation
[P:1]([Cl:5])([Cl:4])([Cl:3])=[O:2].Cl.[N:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>>[O:2]=[P:1]([Cl:5])([Cl:4])[Cl:3].[N:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 24813Phosphorus oxychloride

Product 1

HCID 11977100HCID 11977100, compound

Procedure

To a solution of compound AE or AM′ (1.0 equiv.) in pyridine under argon atmosphere and cooled at −20° C./0° C., the selected amine (5.0 equiv.) and phosphorus oxychloride (1.5 equiv) were successively added. After 30-40 min at 0° C., the reaction was treated with HCl 1M and extracted with AcOEt. The organic layer was washed with brine, dried over MgSO4 and concentrated under reduced pressure. Purification by flash-chromatography afforded the product.

Workup

  1. extractionextracted with AcOEt
  2. washThe organic layer was washed with brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. customPurification by flash-chromatography
  6. customafforded the product

Sources & evidence

ORD record
ord-e38e585ebdf3464ba7c705cad344e002
Source dataset
uspto-grants-2015_05
Patent number
US09029393B2

Reaction notes

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