Hydrochloric Acid → HCID 86628603, compound

A solution of 10 (6.50 g, 11.8 mmol) in conc. HCl (100 mL) is heated to reflux for 18 h. The mixture is cooled to room temperature, washed with EtOAc (2×20 mL) and the aqueous solution is concentrated in vacuo to a brown residue (10 mL). The crude material is loaded on a Amberlite IRA-400 (Cl) resin column (150 mL), wherein the column is preeluted with 6 M HCl (600 mL) and rinsed with H2O (1 L) to pH 6˜7. The column is eluted with water (3 L) and concentrated in vacuo to give a brown solid, which is dissolved in 6 M HCl (40 mL) and added with activated carbon (1.5 g) and heated to reflux for 5 min, cooled to 50° C., filtered through Celite and the filtrate is concentrated in vacuo to give 1 as a pale yellow solid (2.68 g 71%).

1. temperatureto reflux for 18 h
2. washwashed with EtOAc (2×20 mL)
3. concentrationthe aqueous solution is concentrated in vacuo to a brown residue (10 mL)
4. washrinsed with H2O (1 L) to pH 6˜7
5. washThe column is eluted with water (3 L)
6. concentrationconcentrated in vacuo
7. customto give a brown solid, which
8. additionadded with activated carbon (1.5 g)
9. temperatureheated
10. temperatureto reflux for 5 min
11. temperaturecooled to 50° C.
12. filtrationfiltered through Celite
13. concentrationthe filtrate is concentrated in vacuo

ORD record

ord-c10dc7800c094ddc9a7e767a6158d052

Source dataset

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07781418B2