HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 66635626, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Ethyl isocyanate | HCID 8022 | — |
| Reactant | HCID 66635640 | HCID 66635640 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 66635626 | HCID 66635626 | — |
Reaction Steps
5 mg (42 μmol) of 4-N,N-dimethylaminopyridine and 66 μl (0.84 mmol) of ethyl isocyanate were added to a solution of 134 mg (0.42 mmol) of the compound of Example 17A in 2.5 ml of pyridine. The mixture was stirred at RT overnight. A further 66 μl of ethyl isocyanate were then added, and the mixture was heated at 50° C. for 24 h. After cooling to RT, 0.5 ml of ammonia solution (35% in water) was added. The volatile components were removed on a rotary evaporator. A little acetonitrile and 1 N hydrochloric acid were added to the residue, and the solution was separated by preparative HPLC [Method 9]. This gave 110 mg (67% of theory) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09180120B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-81a52b2659724d7faa448f297ee5dd4b |
| Source note | uspto-grants-2015_11 |