HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 11780885, compound → HCID 131721277, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 11780885 | HCID 11780885 | — |
| Reactant | Di-benzoyl-d-tartaric acid | HCID 12362977 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 131721277 | HCID 131721277 | 72.5% |
Reaction Steps
A mixture of (±)-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-piperidinone (1.60 g, 5.73 mmoles) and dibenzoyl-D-tartaric acid (2.28 g, 315 mmol) in 10 mL of methanol was heated at reflux temperature under argon atmosphere and it was cooled to room temperature. After stirring overnight at room temperature the precipitated solid was filtered, washed with a small amount of methanol to obtain the first crop of (R)-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-piperidinone dibenzoyl-D-tartaric acid salt (2.65 g). The filtrate solution was concentrated to a volume of ca 6 mL and was stirred at ambient temperature for one day. The second crop of the chiral salt (0.24 g) was obtained by filtering the solid and washed it with a small amount of methanol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05908934 |
| Source dataset | uspto-grants-1999_06 |
| ORD ID | ord-9445d843b76f42ad8bfa7780195a4b8f |
| Source note | uspto-grants-1999_06 |