HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 59515907, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 5-nitro-1H-isochromen-1-one | HCID 10012760 | — |
| Reactant | Tert-butyl 3-(aminomethyl)azetidine-1-carboxylate | HCID 10679125 | — |
| Product | HCID 59515907 | HCID 59515907 | — |
Reaction Steps
Into a round bottom flask was combined 5-nitro-isochromen-1-one (0.5 g, 0.002 mol), tert-butyl 3-(aminomethyl)azetidine-1-carboxylate (0.975 g, 0.00523 mol), methanol (15 mL, 0.37 mol), and the mixture was heated at reflux for 2 hours. The mixture was cooled to room temperature. LC-MS showed that the starting material was completely consumed. Volatiles were removed and the resulting oil was purified by silica-gel twice in a methanol:methylene chloride (0-10%) gradient and in a EtoAc:Hexane(30-80%). A light yellow solid was obtained (0.56 g). m/z=360.0 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07816371B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-74bc5b1fd559482c8f030d4b7193f268 |
| Source note | uspto-grants-2010_10 |