HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9956467, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Benzyloxybenzyl chloride | HCID 70042 | — |
| Reactant | HCID 363110 | HCID 363110 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 9956467 | HCID 9956467 | 97.1% |
Reaction Steps
To a stirred solution of 2-benzoyl-1,3,4,9-tetrahydro-2H-pyrido[3,4-b]indole (17.75 g, 58.0 mmole) in dry DMF (75 mL) at 5° C. was added 60% NaH (2.78 g, 69.6 mmole). After 10 min, 4-benzyloxybenzyl chloride (14.85 g, 63.8 mmole) was added and the reaction was allowed to warm to RT and stir for 12 hr. The reaction contents were poured into H2O (150 mL) and extracted with EtOAc (2×150 mL). The combined organic phases were washed sequentially with H2O and brine, then were dried over Na2SO4. Concentration under reduced pressure and purification on silica (hexanes/EtOAc, 1:1) afforded the title compound (26.61 g, 97%) as a white solid: MS (ES) m/e 473 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06573272B1 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-eb866264e304413280f2491be91c4824 |
| Source note | uspto-grants-2003_06 |