HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hexamethyldisilazide → HCID 25005526, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | 3,5-Dichloro-4-methylpyridine | HCID 10953827 | — |
| Reactant | HCID 59286715 | HCID 59286715 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 25005526 | HCID 25005526 | — |
Reaction Steps
Following the general procedure, condensation of 3,5-dichloro-4-methylpyridine (93 mg, 0.58 mmol) with compound 522 (150 mg, 0.44 mmol) in THF (2 mL) in the presence of LiHMDS (1.3 mL, 1.3 mmol) afforded compound 129 as a white solid material after purification by column chromatography (55-60% EtOAc in light petroleum). LC-MS: RT=3.95 min.; m/z 468.19, 470.23 (M+H)+, 466.36, 468.33 (M−H)−. 1H NMR (DMSO-d6): δ 8.65 (2H, s), 7.42 (1H, d, J 8.8), 6.89 (1H, d, J 9.1), 4.63 (2H, s), 4.33 (2H, s), 4.08 (2H, s), 3.84 (3H, s), 3.82 (4H, s), 1.39 (3H, s), 1.37 (3H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338431B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-e2501468134e4c33bc46a50666952b4b |
| Source note | uspto-grants-2012_12 |