HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Ammonium Acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 2-[[5-[[(2,3-Difluorophenyl)methyl]thio]-2-methoxythiazolo[4,5-d]pyrimidin-7-yl]amino]-2-methyl-1,3-propanediol | HCID 69060496 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | Ammonium Acetate | HCID 517165 | 0.1% |
| Product | 5-[[(2,3-Difluorophenyl)methyl]thio]-7-[[2-hydroxy-1-(hydroxymethyl)-1-methylethyl]amino]-thiazolo[4,5-d]pyrimidin-2(3H)-one | HCID 11742517 | — |
Reaction Steps
The product from step (g) (0.3 g) was suspended in a mixture of dioxan (50 ml) and conc.HCl (1 ml). Water (1 ml) was added and the resultant solution heated at 60° C. for 12 hours. Allowed to stand over weekend. Solvents removed in vacuo and residue taken up in water. Yellow precipitate collected by filtration and washed with water. Purified using prep. Hplc Acetonitrile: 0.1% ammonium acetate (90:10 to 95:5) over 25 minutes to give 0.063 g of the desired product. 22% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07585867B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-2ec21248001442dd86fe37ff21149857 |
| Source note | uspto-grants-2009_09 |