HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosuccinimide → 7-Chloro-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | 3-(Piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-one | HCID 11379587 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | 7-Chloro-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one | HCID 58181154 | — |
Reaction Steps
801 mg (6.0 mmol) N-chlorosuccinimide were added to 1.23 g (5.0 mmol) 3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one in 10 mL carbon tetrachloride and the reaction mixture was refluxed for 3 days. The solvent was evaporated down using the rotary evaporator and the residue was purified by flash chromatography. The product fractions were combined and the solvent was eliminated using the rotary evaporator. For further purification the product fractions were purified by preparative HPLC. The product fractions were combined and evaporated to dryness using the rotary evaporator.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08829006B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-bb48cb87e0fe4ab7920c78ae22c3ec23 |
| Source note | uspto-grants-2014_09 |