HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisobutylaluminum hydride → HCID 21935886, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisobutylaluminum hydride | HCID 14487 | — |
| Reactant | HCID 67072210 | HCID 67072210 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21935886 | HCID 21935886 | — |
Reaction Steps
0.585 g (2.07 mmol) of the above synthesized 5-(4-trifluoromethyl-phenyl)-pyrazine-2-carboxylic acid methyl ester in 10 ml of abs. THF was cooled down to −30° C. and reacted with 5.18 ml of DIBAL-H-solution (1.2 M in toluene, 3 eq.) for 10 min. The reaction was warmed up during 2.5 h to 10° C. and stirred 1 h at RT. Careful quenching at 0° C. with saturated NaCl solution, twofold extraction with ether, washing with brine, drying over sodium sulfate, and evaporation of the solvents left a crude product which was purified by flash chromatography (SiO2, heptane/AcOEt=4/1) to deliver finally 0.325 g of the title compound as yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115611B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-8d5a65766a9f4c49b8cf29c4e6d02b3b |
| Source note | uspto-grants-2006_10 |