HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hexamethyldisilazide → HCID 25005525, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | 3,5-Dichloro-4-methylpyridine | HCID 10953827 | — |
| Reactant | HCID 59286725 | HCID 59286725 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 25005525 | HCID 25005525 | — |
Reaction Steps
Following the general procedure, condensation of 3,5-dichloro-4-methylpyridine (59 mg, 0.36 mmol) with compound 520 (85 mg, 0.28 mmol) in THF (1.5 mL) in the presence of LiHMDS (0.85 mL, 0.85 mmol) afforded compound 127 as a white solid material after purification by column chromatography (60-70% EtOAc in light petroleum). LC-MS: RT=3.70 min.; m/z 438.21, 440.21 (M+H)+, 436.30, 438.27 (M−H)−. 1H NMR (DMSO-d6): δ 8.65 (2H, s), 7.42 (1H, d, J 8.9), 6.87 (1H, d, J 9.0), 4.63 (2H, s), 4.25 (2H, s), 4.07 (2H, s), 3.84 (3H, s), 3.64 (4H, t, J 5.3), 1.60 (4H, t, J 5.3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338431B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-8e7678b39d3f4f129b2d47d3761938f0 |
| Source note | uspto-grants-2012_12 |