HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 59233185, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 59233051 | HCID 59233051 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 59233185 | HCID 59233185 | — |
Reaction Steps
A solution of diethyl 2-(6-chloropyridazin-3-yl)-2-methylmalonate (19.8 g, 69.1 mmol) and LiOH (3.31 g, 138 mmol) in MeOH:Water (3:1, 200 mL) was stirred at 25° C. for 3 hrs. MeOH was removed from the reaction via rotary evaporation, and the resulting residue was reconstituted in H2O (300 mL). The aqueous mixture was washed with Et2O (3×100 mL) and then lyophilized to dryness to provide lithium 2-(6-chloropyridazin-3-yl)propanoate 48B in quantitative yield. The material was used without further work-up. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.36 (3 H, d, J=7.33 Hz) 3.63 (1 H, q, J=7.24 Hz) 7.71 (2 H, s). ESI-MS:m/z 187.0 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178534B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-f5de37a5cf0a4dea941914518b88a4a9 |
| Source note | uspto-grants-2012_05 |