HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 16736110, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 11176568 | HCID 11176568 | — |
| Reactant | Trimethylaluminum | HCID 16682925 | — |
| Catalyst | HCID 178420554 | HCID 178420554 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 16736110 | HCID 16736110 | — |
Reaction Steps
A suspension of 6-chloro-9-(2-chloro-3,4,5-trimethoxy-benzyl)-9H-purin-2-ylamine, see example 97) (0.2 mmol) and tetrakis(triphenylphosphino)-palladium (0.02 mmol) in dry THF (3 mL) was treated with trimethylaluminum (2M in toluene, 0.45 mmol) under nitrogen and heated to reflux for 3 h. The reaction mixture was cooled to r.t., diluted with toluene (5 mL) and quenched with methanol (0.5 mL) followed by ammonium chloride (1 mmol). The mixture was heated to reflux for 2 h and filtered, while hot, on Celite. See J. Med. Chem. 1999, 42, 2064–2086. TLC (100% EtOAc) Rf was 0.2. HPLC Rt: 4.800 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07138401B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-c0bd738012a54a28a30480153156c942 |
| Source note | uspto-grants-2006_11 |