HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium borohydride → HCID 69023059, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 69023509 | HCID 69023509 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 69023059 | HCID 69023059 | 33.1% |
Reaction Steps
A mixture of intermediate (16) (0.0848 mol) in methanol (400 ml) was cooled to 10° C. sodium tetrahydroborate (0.102 mol) was added portionwise. The mixture was stirred at room temperature for 2 hours, poured out into ice water and extracted with DCM. The organic layer was separated, washed with water, dried (MgSO4), filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 95/5/0.1; 20–45 μm). The pure fractions were collected and the solvent was evaporated, yielding 12.3 g (33%) of 2-amino-α-(3-chlorophenyl)-5-[(4-chlorophenyl)(1-methyl-1H-imidazol-5-yl)methyl]-benzenemethanol (intermediate 17).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07153958B2 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-2da3bc96b94f48fd84f7bc40a55f0a67 |
| Source note | uspto-grants-2006_12 |