Hydrochloric Acid → HCID 23446892, compound

Temperature

120 °C

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

1. additionwere added at 22 to 30° C.
2. concentrationthe mixture was then concentrated in vacuo
3. additionThe residue was treated with 150 ml of phosphorus oxychloride
4. concentrationThe reaction mixture was then concentrated in vacuo
5. dissolutionthe residue was dissolved in methylene chloride
6. additionthe solution was treated with water
7. customAfter the phase separation
8. washthe organic phase was again washed with water
9. dry with materialwith saturated sodium chloride solution, and dried over magnesium sulfate
10. concentrationAfter concentration, 2.4 g (48% of theory) of the title compound
11. customwere obtained as a yellowish powder of m.p. 77-80° C.

ORD record

ord-8479d47b6bc3457cbc42a520fb41b705

Source dataset

uspto-grants-2004_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06683213B1