HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dibenz(b,f)azepine → (Z)-2-(5H-dibenzo[b,f]azepin-5-yl)acetonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dibenz(b,f)azepine | HCID 9212 | — |
| Reactant | Bromoacetonitrile | HCID 11534 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Bis(tetrabutylammonium) sulphate | HCID 11433187 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (Z)-2-(5H-dibenzo[b,f]azepin-5-yl)acetonitrile | HCID 11345294 | 51.7% |
Reaction Steps
(Z)-5H-dibenzo[b,f]azepine (0.1 g, 0.5 mmol), tetrabutylammonium sulfate (0.35 g, 1.0 mmol), 2-bromoacetonitrile (0.4 mL, 5.0 mmol) and 50% aqueous sodium hydroxide (1 mL) were mixed in DCM (1 mL) and the reaction mixture was stirred for 5 days. The mixture was diluted in water and the aqueous layer was extracted with DCM (2 times). The combined organic layers were dried over sodium sulfate, filtered and concentrated. The crude product was purified by flash chromatography (0% to 50% ethyl acetate in hexanes) to afford title compound 365 (60 mg, 50%). 1H NMR (CDCl3) δ (ppm): 7.36-7.31 (m, 2H), 7.26-7.23 (m, 2H), 7.17-7.11 (m, 4H), 6.76 (s, 2H), 4.47 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09193749B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-4b2c20dccdb047869b6e8d496f3d08b3 |
| Source note | uspto-grants-2015_11 |