HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 178438391, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 12862372 | HCID 12862372 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178438391 | HCID 178438391 | 55.8% |
Reaction Conditions
| Temperature | 124 °C |
|---|
Reaction Steps
A mixture of 5.1 g (0.01894 mol) of 2-(1-methylethyl)-4-oxo-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidine-7-carbonitrile (Example 16), 6.5 g (0.1 mol) of sodium azide and 5.35 g (0.1 mol) of ammonium chloride in 150 ml of dimethylformamide is stirred and heated at 124° C. for twenty-two hours under nitrogen. The reaction mixture is cooled, filtered and the filtrate evaporated. The residue is treated with 1 l water and acidified with concentrated hydrochloric acid. The resulting precipitate is collected, suspended in hot water, the suspension cooled and filtered to give 3.3 g of 2-(1-methylethyl)-7-(1H-tetrazol-5-yl)-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidin-4-one; mp 288° C. (dec) after recrystallization from pyridine-ethanol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04332947 |
| Source dataset | uspto-grants-1982_06 |
| ORD ID | ord-aa3209e4bc824adf9c4f1ede8b43e5e2 |
| Source note | uspto-grants-1982_06 |