HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → 3-(3H-Isobenzofuran-1-ylidene)-1-piperidin-1-ylmethyl-1,3-dihydro-indol-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | 3-(2-Benzofuran-1(3H)-ylidene)-1,3-dihydro-2H-indol-2-one | HCID 68779381 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 3-(3H-Isobenzofuran-1-ylidene)-1-piperidin-1-ylmethyl-1,3-dihydro-indol-2-one | HCID 68835801 | 62.2% |
Reaction Steps
A mixture of 3-(3H-isobenzofuran-1-ylidene)-1,3-dihydro-indol-2-one (4.32 g, 17.3 mmol), paraformaldehyde (0.99 g, 32.9 mmol), and piperidine (2.14 mL, 21.7 mmol) in 192 mL EtOH and 48 mL dioxane was heated at reflux for 18.5 h. The solution was concentrated in vacuo to a volume of 100 mL and then refluxed for 1 h to dissolve the precipitant. The mixture was allowed to cool to room temperature and the precipitate filtered to give the title compound (3.728 g) as a bright yellow solid. An additional 0.52 g of the title compound was obtained by crystallization of the filtrate from ethyl acetate. The two lots were combined to give 4.248 g (71%) of the title compound as a bright yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06699863B1 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-d6d1ad98c2dc4060a057b4e3d87c0662 |
| Source note | uspto-grants-2004_03 |