HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 67010052, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 67009927 | HCID 67009927 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67010052 | HCID 67010052 | 108.3% |
Reaction Steps
Under a nitrogen gas stream, 0.75 g (20 mmol) of lithium aluminum hydride was added to tetrahydrofuran (70 mL) under ice cooling, and a tetrahydrofuran (30 mL) solution of 2.3 g (9.9 mmol) of methyl 2-(5-methyl-3-isoxazolyl)aminonicotinate was added dropwise to the above solution. The resulting mixture was stirred for one hour under ice cooling. Ethyl acetate was added to the reaction mixture, and 8.0 mL of a 10% aqueous solution of sodium hydroxide was further added thereto. Insoluble materials were filtered off. The filtrate was concentrated, and the residue was dissolved in ethyl acetate, dried, filtered, and concentrated. Thus, 2.2 g of the title compound was obtained as an orange-colored viscous product (yield: quantitative).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08334236B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-6fb22c65001b452996c206519050bd2b |
| Source note | uspto-grants-2012_12 |