HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → HCID 135736099, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 23117142 | HCID 23117142 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 135736099 | HCID 135736099 | 62.4% |
Reaction Steps
6-(tetrahydro-2H-pyran-2-yloxy)-3-[4-(tetrahydro-2H-pyran-2-yloxy)benzyl]-1,2-benzisoxazole (3.85 mmol) and paratoluenesulfonic acid (APTS, catalytic amount) were dissolved in methanol (20 ml). After reaction at 60-70° C. for 3 h, the reaction mixture was cooled to room temperature and poured into saturated NaHCO3 and extracted with EtOAc. After washing (H2O) and drying (MgSO4), the extract was concentrated. The crude product was purified by flash chromatography (toluene/1,4-dioxane 8/2) and crystallised to give an off-white crystal (0.58 g, 31%). mp 178° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977364B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-42bc5f1ff95a47359b14530720846d90 |
| Source note | uspto-grants-2011_07 |