HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzophenone imine → 3-(Benzhydrylidene-amino)-1-methyl-pyrrolidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzophenone imine | HCID 136809 | — |
| Reactant | 3-Amino-1-methylpyrrolidin-2-one | HCID 45791133 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | 3-(Benzhydrylidene-amino)-1-methyl-pyrrolidin-2-one | HCID 89648998 | — |
Reaction Steps
Benzophenone imine [CAS: 1013-88-3] (16.67 g, 91.98 mmol) was added dropwise to a solution of 3-amino-1-methylpyrrolidine-2-one [CAS 119329-48-5] (10 g, 87.60 mmol) in DCE (100 mL) under N2 and the reaction was heated at reflux for 18 hours. The solvent was evaporated to afford an amber oil. This was purified using flash silica in a large sinter funnel, eluting with 4:1 to 3:7 i-hexane:EtOAc. An incomplete separation was achieved. 3-(Benzhydrylidene-amino)-1-methyl-pyrrolidin-2-one (D1) was isolated (25 g) with approximately 11% of an impurity present, but was used in the next step without further purification;
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09309254B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-47c8073d19b94c70913f6f2748c967cc |
| Source note | uspto-grants-2016_04 |