HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-[3-(1-Benzhydryl-2-methyl-1H-indol-3-yl)-propyl]-benzoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Bromodiphenylmethane | HCID 236603 | — |
| Reactant | 4-[3-(2-Methyl-1H-indol-3-yl)-propyl]-benzoic acid methyl ester | HCID 67055494 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-[3-(1-Benzhydryl-2-methyl-1H-indol-3-yl)-propyl]-benzoic acid methyl ester | HCID 67055500 | — |
Reaction Steps
To a solution of the product from step 2 (1.66 g, 4.86 mmol) in DMF (20 mL) was added NaH (60% in mineral oil, 0.24 g, 5.83 mmol) under N2 atmosphere. The mixture was stirred for 1 h at room temperature, followed by the dropwise addition of benzhydryl bromide (1.8 g, 7.29 mmol) in DMF (5 mL). This reaction mixture was stirred overnight at room temperature. Water (500 mL) was added to reaction mixture, it was extracted with EtOAc, washed with brine, dried (Na2SO4), and concentrated under reduced pressure to a brown syrup, which was purified by silica-gel chromatography using 10% EtOAc/hexanes as eluent to isolate 4-[3-(1-Benzhydryl-2-methyl-1H-indol-3-yl)-propyl]-benzoic acid methyl ester as a white solid in 76% (1.47 g) yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07906548B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-c49dc22e808342f089825e41b9fb4cb8 |
| Source note | uspto-grants-2011_03 |