HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hexamethyldisilazide → HCID 25005889, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | 3,5-Dichloro-4-methylpyridine | HCID 10953827 | — |
| Reactant | HCID 59286717 | HCID 59286717 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 25005889 | HCID 25005889 | — |
Reaction Steps
Following the general procedure, condensation of 3,5-dichloro-4-methylpyridine (154 mg, 0.95 mmol) with compound 526 (250 mg, 0.73 mmol) in THF (4 mL) in the presence of LiHMDS (2.2 mL, 2.2 mmol) afforded compound 132 as a white solid material after purification by column chromatography (45-55% EtOAc in light petroleum). LC-MS: RT=4.39 min.; m/z 472.15, 474.14 (M+H)+. 1H NMR (DMSO-d6): δ 8.65 (2H, s), 7.42 (1H, d, J 8.9), 6.88 (1H, d, J 8.9), 4.64 (2H, s), 4.43 (2H, s), 4.24 (2H, s), 3.85 (3H, s), 3.84 (2H, s), 2.91 (4H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338431B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-2c68965f58a345bb933473cc2fbb0c46 |
| Source note | uspto-grants-2012_12 |