Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 66635083 | HCID 66635083 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66614413 | HCID 66614413 | — |
Reaction Steps
133 mg (0.26 mmol) of the compound from example 65A were initially charged in dimethylformamide (1.4 ml), then 213 mg (1.32 mmol) of N,N-carbonyldiimidazole and 0.44 ml (3.16 mmol) of triethylamine were added and the mixture was stirred at 100° C. overnight. Thereafter, another 200 mg (1.23 mmol) of N,N-carbonyldiimidazole were added and the mixture was again stirred at 100° C. overnight. The reaction mixture was purified directly by means of preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid gradient). This gave 79 mg (68% of theory) of the title compound in solid form.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09096592B2 |
|---|
| Source dataset | uspto-grants-2015_08 |
|---|
| ORD ID | ord-d8efb322f3454db2b572492f8b30246f |
|---|
| Source note | uspto-grants-2015_08 |
|---|