HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 12133110, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Phenoxypyrimidine-4-carbonyl chloride | HCID 12970158 | — |
| Reactant | 2-(4-Fluorophenyl)-1-(4-morpholin-4-yl-pyrazolidin-1-yl)ethanone | HCID 21992206 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Water methylene chloride | HCID 21908982 | — |
| Product | HCID 12133110 | HCID 12133110 | 23% |
Reaction Steps
2-Phenoxypyrimidine-4-carbonyl chloride, 18, (0.07 g, 0.28 mmol) in methylene chloride (1.5 mL) is added dropwise to a suspension of 2-(4-fluorophenyl)-1-(4-morpholin-4-yl-pyrazolidin-1-yl)ethanone, 13, (0.06 g, 0.18 mmol) in a 2:5 water/CH2Cl2 solution (7 mL) containing NaOH (0.0112 g, 0.28 mmol) at room temperature. The solution is stirred 18 hours and diluted with additional 2:5 water/CH2Cl2. The layers are allowed to separate and the aqueous phase extracted with additional methylene chloride. The organic layers are combined, dried, filtered and concentrated in vacuo to afford a tan solid which is purified by preparative HPLC to provide 0.021 g (23% yield) of the desired product as an oily solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06960593B2 |
| Source dataset | uspto-grants-2005_11 |
| ORD ID | ord-3e3df849b87b4485bb561ac600e0303b |
| Source note | uspto-grants-2005_11 |