HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 84766583, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Reactant | HCID 90022261 | HCID 90022261 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 84766583 | HCID 84766583 | 98.4% |
Reaction Steps
A solution of LiBH4 (2M in THF, 6.28 mL, 12.6 mmol) was added to a solution of methyl 2,4-difluoro-6-methoxybenzoate (1.15 g, 5.71 mmol) in THF (30 mL). The solution was stirred at rt for 23 h, then at 60° C. for 4.5 h, and reflux for 18.5 h. After cooling to rt, H2O (20 mL) was added dropwise and the mixture stirred for 5 min before being partially concentrated in vacuo. DCM (20 mL) was added, the phases were separated, and the aqueous phase was extracted with DCM (2×10 mL). The organic layers were concentrated in vacuo to yield the title compound (978 mg, 5.62 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09249160B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-27396ec92ac1413fb8c59b05b10273a0 |
| Source note | uspto-grants-2016_02 |