HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-methyl-2-pyrrolidone → HCID 58277336, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | HCID 58277324 | HCID 58277324 | — |
| Catalyst | Zinc cyanide (Zn(CN)2) | HCID 11186 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Product | HCID 58277336 | HCID 58277336 | — |
Reaction Conditions
| Temperature | 200 °C |
|---|
Reaction Steps
100 mg (0.236 mmol) of the compound of Example 51A are provided in 1 ml of 1-methyl-2-pyrrolidone, 55.4 mg (0.472 mmol) of zinc cyanide and 27.3 mg (0.024 mmol) of tetrakis(triphenylphosphine)palladium(0) are added, and the mixture is heated in a closed glass vessel at 200° C. under microwave irradiation for 30 min. The reaction mixture is subsequently filtered through kieselguhr and eluted with methanol, the filtrate is rendered weakly acidic with a 1N aqueous hydrogen chloride solution and concentrated, and the residue is purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient). 33 mg (34% of theory) of the title compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399682B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-9020e46667cb40e3ae9ea6c5d03221c4 |
| Source note | uspto-grants-2013_03 |