HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium borohydride → 3-Benzyl-1,2,3,4,5,6-hexahydro-7h-pyrido[3,4-d][2]benzazepin-7-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 3-Benzyl-7-oxo-6,7-dihydro-5h-pyrido[3,4-d][2]benzazepin-3-ium bromide | HCID 67247773 | — |
| Solvent | Water ethanol | HCID 19096565 | — |
| Product | 3-Benzyl-1,2,3,4,5,6-hexahydro-7h-pyrido[3,4-d][2]benzazepin-7-one | HCID 59548522 | — |
Reaction Steps
To a suspension of Example 180E (17.7 g, 46.4 mmol) in 200 mL of ethanol/water (4:1) at 0° C. was added NaBH4 (8.9 g, 0.232 mol) portion-wise. After stirring for 0.5 hour, the mixture was quenched with 1 N HCl to pH 4-5 and concentrated under reduced pressure. The residue was dissolved in 100 mL of saturated aqueous K2CO3 and extracted with dichloromethane. The organic phase was washed with brine, dried and purified by column chromatography on silica gel eluting with dichloromethane/methanol (30:1) to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08546377B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-dfc17fbe992e4893892e01946691a99d |
| Source note | uspto-grants-2013_10 |