HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 131733671, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | 5-Chloro-2-methyl-2,3,3a,12b-tetrahydrodibenzo(2,3:6,7)oxepino(4,5-c)pyrrole | HCID 9903970 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 131733671 | HCID 131733671 | 80% |
Reaction Steps
500 mg Asenapine free base (˜1.7 mmol) were dissolved in 1.0 ml acetone and 320 mg of citric acid (Fluka #24788) which was dissolved in 1.0 ml water was added to the solution containing the free base. This solution was then seeded with a few mg of crystalline citrate salt according to example 1 and to the very thin suspension 2.0 ml water was added and stirred was performed while keeping the vial open letting some acetone evaporate. On the next day the obtained suspension was filtered and about 633 mg of solid product was obtained after drying under vacuum at r.t. for about 18 hours. Powder X-ray diffraction of the obtained solid product showed that the same crystalline form as in example 1 was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169262B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-7a2f6ceab71344e7aa65f7c65c7f3a22 |
| Source note | uspto-grants-2015_10 |