HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisobutylaluminum hydride → HCID 21935665, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisobutylaluminum hydride | HCID 14487 | — |
| Reactant | HCID 67072262 | HCID 67072262 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21935665 | HCID 21935665 | — |
Reaction Steps
1.250 g (3.717 mmol) of the above prepared 4-cyclopropyl-2-(3-trifluoromethyl-phenyl)-pyrimidine-5-carboxylic acid ethyl ester in 19 ml of abs. THF was cooled down to −15° C. and reacted with 11.2 ml of DIBAL-H-solution (1.0 M in toluene, 3 eq.) for 1/2 h. Careful quenching with ice/HCl dil., twofold extraction with AcOEt, washing with water, drying over sodium sulfate, and evaporation of the solvents left a crude product which was purified by flash chromatography (SiO2, hexane/AcOEt=1/1l) to yield finally 1.096 g of the title compound as white solid of mp. 108–09° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115611B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-700a6c671422465bac87edfe458f867a |
| Source note | uspto-grants-2006_10 |