Hydrochloric Acid → HCID 23446892, compound

With stirring, 1.18 g (0.033 mol) of hydrogen chloride, dissolved in 35 ml of diethyl ether, were added to a suspension of 5 g (0.027 mol) of the compound from Example A3 in 50 ml of 1,2-dichloroethane at 22-30° C., and the mixture was then concentrated under reduced pressure. The residue was admixed with 150 ml of phosphorus oxychloride and stirred at 120° C. for 3 h. The reaction mixture was then concentrated under reduced pressure and the residue was dissolved in methylene chloride, admixed with water and neutralized using 2 N aqueous sodium hydroxide solution. Following phase separation, the mixture was once again washed with water and then with saturated sodium chloride solution and dried over magnesium sulfate. Concentration gave 2.4 g (48% of theory) of the title compound as a yellowish powder of m.p. 77-80° C.

1. concentrationthe mixture was then concentrated under reduced pressure
2. stirringstirred at 120° C. for 3 h
3. concentrationThe reaction mixture was then concentrated under reduced pressure
4. dissolutionthe residue was dissolved in methylene chloride
5. customFollowing phase separation
6. washthe mixture was once again washed with water
7. dry with materialwith saturated sodium chloride solution and dried over magnesium sulfate
8. concentrationConcentration

ORD record

ord-62862a596c484180a838a1bad8701e64

Source dataset

uspto-grants-2002_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06472349B1