HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 178478873, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | HCID 178451556 | HCID 178451556 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178478873 | HCID 178478873 | — |
Reaction Steps
To a suspension of tert-butyl 4-(cyclohexylamino)-1-(4-iodophenyl)-2-oxo-1,3,8-triazaspiro[4.5]dec-3-ene-8-carboxylate (10.9 g, 19.7 mmol) in 4N HCl dioxane (99 mL, 395 mmol) was added small amounts of DCM and MeOH to obtain a solution. After stirring at rt for 1 h, the reaction mixture was concentrated in vacuo, the residue was triturated with diethyl ether and the product was isolated as a white solid by filtration. LRMS (M+1)=453. LC analysis and 1H NMR indicate the presence of an unknown (20%), the titled compound was used as is in subsequent steps, allowing for purification at a later stage.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399473B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-642fa9a573684c36ac4563eb26d540d4 |
| Source note | uspto-grants-2013_03 |