HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributyltin Chloride → HCID 178439872, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributyltin Chloride | HCID 15096 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 19383105 | HCID 19383105 | — |
| Product | HCID 178439872 | HCID 178439872 | 51.6% |
Reaction Steps
A mixture of 2-propyl-1-[[2-(2-cyanophenyl)-5-pyridinyl]methyl]-1H-benzimidazole (0.50 g, 1.42 mmol), NaN3 (0.18 g, 2.84 mmol), and tri-n-butyltin chloride (0.92 g, 2.84 mmol) in xylenes (10 mL) was heated under reflux for 48 h. The reaction mixture was concentrated and 2N HCl was added. The mixture was extracted with ether (discarded) and adjusted to pH 5 with 50% NaOH. The aqueous phase was extracted with CH2Cl2, and the extracts were washed with water, dried, and concentrated. Purification by flash chromatography (5% MeOH/CH2Cl2) and trituration with EtOH gave 0.29 g (51%) of product as a white solid, mp 240°-241° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05451583 |
| Source dataset | uspto-grants-1995_09 |
| ORD ID | ord-93afd09932a044af8708f31d110cf6c9 |
| Source note | uspto-grants-1995_09 |