1,4-Dioxane hydrochloride → HCID 67507091, compound

HRID 1829108Notes

Reaction equation

HRID 1829108 reaction equation
[ClH:1].[N+:2]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C@@H:12]2[CH2:16][NH:15][C@H:14]([C:17]([N:19]3[CH2:23][CH2:22][S:21][CH2:20]3)=[O:18])[CH2:13]2)=[CH:7][CH:6]=1)([O-])=O.Cl.O1CCOCC1>C(O)C.[Pd]>[ClH:1].[NH2:2][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C@@H:12]2[CH2:16][NH:15][C@H:14]([C:17]([N:19]3[CH2:23][CH2:22][S:21][CH2:20]3)=[O:18])[CH2:13]2)=[CH:7][CH:6]=1

Participants

5

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67507135HCID 67507135, compound

Product 1

HCID 67507091HCID 67507091, compoundYield 7.1%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

The title compound (200 mg) of Example 55 was dissolved in ethanol (10 mL), and 4 mol/L hydrochloric acid-1,4-dioxane (0.28 mL) and 10% palladium/carbon (100 mg) were added. The mixture was stirred under a hydrogen atomosphere (1 atm) at room temperature for 18 hr. The reaction mixture was filtrated and the filtrate was concentrated under reduced pressure, and the obtained solid was washed with ethanol to give the title compound (13 mg) as a white powder.

Workup

  1. filtrationThe reaction mixture was filtrated
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. washthe obtained solid was washed with ethanol

Sources & evidence

ORD record
ord-d65b8b0114254fd490ea21e7ffd4c0be
Source dataset
uspto-grants-2006_06
Patent number
US07060722B2

Reaction notes

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