HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 18796731, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 18796730 | HCID 18796730 | — |
| Reactant | Diisobutylaluminumhydride | HCID 21225700 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 18796731 | HCID 18796731 | 52% |
Reaction Steps
0.50 g (0.0013 mol) of 2-ethoxycarbonyl-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline was dissolved in a solvent mixture comprising 20 ml of methylene chloride and 20 ml of tetrahydrofuran. 2.6 ml of a 1.0M solution of diisobutylaluminum hydride in toluene was dropped into the solution prepared above at -78° C. under stirring. The obtained mixture was stirred at -78° C. for several hours, followed by the addition of 20 ml of methanol. The obtained mixture was distilled under a reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography and recrystallized from ethyl acetate/n-hexane to give 0.23 g of the title compound as a pale-yellow crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05576322 |
| Source dataset | uspto-grants-1996_11 |
| ORD ID | ord-ca7ea0a4fd67460db8b9c64880fdad4f |
| Source note | uspto-grants-1996_11 |