HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → (1-Tritylindazol-3-yl)methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 66846309 | HCID 66846309 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (1-Tritylindazol-3-yl)methanol | HCID 66846262 | 78.8% |
Reaction Steps
To a solution of the crude isobutyl 1-tritylindazole-3-carboxylate (180 g; 0.39 mol) in THF (1 L) stirred at room temperature was added slowly a suspension of LiAlH4 (18 g; 0.48 mol) in THF (100 ml). Once the addition was complete, the mixture was stirred at room temperature for 30 minutes, and the reaction was then stopped by cooling the mixture to 0° C. and successively adding water (40 ml), 2N NaOH (40 ml) and water (60 ml). The solid thus formed was filtered off and the solution was concentrated under reduced pressure. The crude residue obtained was purified by crystallization from a 1/1 hexane/ethyl acetate mixture. 120 g of (1-tritylindazol-3-yl)methanol were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835481B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-b030748ee7574ed586199bcee441325b |
| Source note | uspto-grants-2014_09 |