HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 59485031, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 59485021 | HCID 59485021 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59485031 | HCID 59485031 | 60.8% |
Reaction Steps
To the methanol (1.0 mL) solution of 1-{4-[4-(2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazin-1-yl]phenyl}ethanone (39 mg, 0.10 mmol) synthesized in Example 95, sodium borohydride (11 mg, 0.30 mmol) was added under ice cooling. The mixture was stirred for 2 hours. The reaction solution was added with water, and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate. The solvent was removed by distillation under reduced pressure. The resulting residue was crystallized from hexane to obtain the title compound 24 mg (yield 60%). Melting point was 133 to 136° C. (hexane-ethyl acetate).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288390B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-84ac5e3b6d744f68b91813535033f102 |
| Source note | uspto-grants-2012_10 |