1,4-Dioxane hydrochloride → HCID 21201993, compound

HRID 1979301Notes

Reaction equation

HRID 1979301 reaction equation
[C:1]([C:5]([CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[N:12]([C:19](=[O:24])[C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:11][CH:10]([NH:25]C(OC(C)(C)C)=O)[C:9]1=[O:33])=[O:6])([CH3:4])([CH3:3])[CH3:2].Cl.O1CCOCC1>C(Cl)(Cl)Cl>[C:1]([C:5]([CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[N:12]([C:19](=[O:24])[C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:11][CH:10]([NH2:25])[C:9]1=[O:33])=[O:6])([CH3:4])([CH3:2])[CH3:3]

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 21201739HCID 21201739, compound

Product 1

HCID 21201993HCID 21201993, compoundYield 92.1%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Conditions

Temperature
50 °C

Procedure

1-tert-Butylcarbonylmethyl-2-oxo-3-tert-butoxycarbonylamino-5-pivaloyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (1 g) was dissolved in chloroform (10 ml), 4N HCl-dioxane (5 ml) was added to the solution, and the mixture was stirred at 50° C. for one hour. After the reaction mixture was allowed to cool, crystals so precipitated were collected by filtration. The crystals were neutralized with saturated aqueous sodium bicarbonate, and extracted with methylene chloride, dried over anhydrous sodium sulfate, to thereby obtain 720 mg of the titled compound (Yield: 92%).

Workup

  1. temperatureto cool
  2. customcrystals so precipitated
  3. filtrationwere collected by filtration
  4. extractionextracted with methylene chloride
  5. dry with materialdried over anhydrous sodium sulfate

Sources & evidence

ORD record
ord-3b5df22d0ca64d168829e0a50d9f27ea
Source dataset
uspto-grants-2001_05
Patent number
US06239131B1

Reaction notes

Loading…