HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → Tert-butyl 1-(tetrahydrofuran-3-yl)azetidin-3-ylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 3-Oxotetrahydrofuran | HCID 529392 | — |
| Reactant | 3-Aminoazetidine, 3-BOC protected | HCID 1519405 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Tert-butyl 1-(tetrahydrofuran-3-yl)azetidin-3-ylcarbamate | HCID 67126577 | — |
Reaction Steps
Tert-butyl azetidin-3-ylcarbamate (0.550 g), dihydrofuran-3(2H)-one (0.412 g) and sodium triacetoxyborohydride (1.015 g) were stirred together in dichloromethane (5 mL). After stirring overnight, the reaction was poured into saturated aqueous NaHCO3 solution (25 mL) and extracted with dichloromethane (50 mL). The organic layer was washed with brine (25 mL), dried over magnesium sulfate, filtered, and concentrated. Silica gel chromatography (GraceResolv 12 g) eluting with a gradient of 0.5% to 7.5% methanol/dichloromethane over 30 minutes gave tert-butyl 1-(tetrahydrofuran-3-yl)azetidin-3-ylcarbamate. The resulting material was treated with HCl/dioxane for 1 hour, and then concentrated to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09174982B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-61d00c48f6f3411fa98ae7b0c139def9 |
| Source note | uspto-grants-2015_11 |