HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → (4-Hydroxy-[1,4']bipiperidinyl-1'-yl)-(3-methanesulfonyl-phenyl)-methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Methanesulfonylbenzoic acid | HCID 220380 | — |
| Reactant | PyBroP | HCID 2733179 | — |
| Reactant | 1-(4-Piperidinyl)-4-piperidinol dihydrochloride | HCID 22397506 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (4-Hydroxy-[1,4']bipiperidinyl-1'-yl)-(3-methanesulfonyl-phenyl)-methanone | HCID 22397427 | 87.4% |
Reaction Steps
PyBrOP™ (25.3 g) was added to a stirred solution of 3-methanesulphonyl benzoic acid (10 g), [1,4′]bipiperidinyl-4-ol dihydrochloride (13 g, see Method D) and Hunig's base (34 ml) in dichloromethane (500 ml). The resulting mixture was stirred at RT overnight, then washed with saturated NaHCO3 solution (300 ml) followed by saturated brine (300 ml). The organic layer was dried (MgSO4) and evaporated to leave an oily residue. Column chromatography (silica, 20% methanol in DCM) gave the product as a white solid (16 g; MS: APCI+(M+H) 367).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07179922B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-fc83791b8c8c4d4ebdd846daa39b6290 |
| Source note | uspto-grants-2007_02 |