HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86282690, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 90465074 | HCID 90465074 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86282690 | HCID 86282690 | 63% |
Reaction Steps
1 g of LiBH(Et)3 (1.12 mmol, 1.33 eq, 1M solution in THF) is added to a solution of 7,8-dimethoxy-3-(4-methoxybenzyl)-1H-3-benzazepine-2,4(3H,5H)-dione (300 mg, 0.84 mmol) in THF (4.5 mL) at −78° C. The reaction mixture is held at that temperature for 1 hour 30 minutes with stirring and then hydrolysed with saturated aqueous ammonium chloride solution (4 mL). After a slow return to ambient temperature, 2 mL of water and 5 mL of dichloromethane are introduced, the aqueous phase is extracted with 10 mL of dichloromethane, and the organic phase is dried. The crude product obtained is purified by flash chromatography on a silica column (dichloromethane/methanol 98/2) to obtain the title product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08927708B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-8f8d30d4b72b4653a4ddf76674ac31c3 |
| Source note | uspto-grants-2015_01 |