HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → Tert-butyl 4-[(6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl)methyl]piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | 6-Hydroxy-3-coumaranone | HCID 235717 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Tert-butyl 4-[(6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl)methyl]piperazine-1-carboxylate | HCID 60155786 | 50.4% |
Reaction Steps
A solution of 6-hydroxybenzofuran-3(2H)-one (3.00 g, 20.0 mmol) in ethanol (20 mL) was added with 1-tert-butoxycarbonylpiperazine (3.73 g, 20.0 mmol), and 37% aqueous formaldehyde (1.62 g, 20.0 mmol) at room temperature. The mixture was stirred overnight at room temperature, and then subjected to suction filtration, and the filtrate was concentrated. Crude product obtained by silica gel column chromatography (hexane/ethyl acetate) was recrystallized from ethyl acetate to obtain the objective tert-butyl 4-[(6-hydroxy-3-oxo-2,3-dihydrobenzofuran-7-yl)methyl]piperazine-1-carboxylate (3.51 g, 50%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09156827B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-d47d30ce2e7148ee8811470a4664c4e1 |
| Source note | uspto-grants-2015_10 |