HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 11784741, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 59514566 | HCID 59514566 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11784741 | HCID 11784741 | 27% |
Reaction Steps
This crude methyl[4-chloro-2-{4-[(4-chlorobenzoyl)(methyl)amino]benzyl}-6-(dimethyl-amino)pyrimidin-5-yl]acetate was dissolved in THF (3 mL) and treated with 1N NaOH (2 mL) and stirred at room temperature for 24 hour. Et2O was added and the organic phase was siphoned off. The remaining aqueous layer was acidified with 6N HCl to pH˜5 and the separated solids were collected by suction and rinsed with water and diisopropyl ether. Drying under high vacuum at room temperature for 4 hours then gave [4-chloro-2-{4-[(4-chlorobenzoyl)(methyl)amino]-benzyl}-6-(dimethylamino)pyrimidin-5-yl]acetic acid (0.029 g, 27% yield) as a pale yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07960393B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-fd6d57117298475f84ac2e942b7eefe5 |
| Source note | uspto-grants-2011_06 |