HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl N-allyl-N-[2-(methoxy(methyl)amino)-2-oxo-ethyl]carbamate → tert-Butyl N-allyl-N-[2-oxo-2-(2-thienyl)ethyl]carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl N-allyl-N-[2-(methoxy(methyl)amino)-2-oxo-ethyl]carbamate | HCID 86697892 | — |
| Reactant | HCID 178418439 | HCID 178418439 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | tert-Butyl N-allyl-N-[2-oxo-2-(2-thienyl)ethyl]carbamate | HCID 86697895 | 56% |
Reaction Steps
To a solution of tert-butyl N-allyl-N-[2-(methoxy(methyl)amino)-2-oxo-ethyl]carbamate (25 g, 96.8 mmol) in tetrahydrofuran (339 mL) at −78° C. is added drop wise 2-thienyllithium (145 ml, 1 M in tetrahydrofuran) over 20 min. The reaction is carefully quenched with aqueous ammonium chloride (20 mL), diluted with water (100 mL), and extracted with dichloromethane. The organic layers are combined, dried over sodium sulfate, filtered, and concentrated to give a residue. The residue is purified by silica gel flash chromatography, eluting with hexane/ethyl acetate (1:0) to hexane/ethyl acetate (5:1) to give the title compound (15.2 g, 56%). ES/MS (m/e): 182 (M+H-100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08889856B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-f68aa4a492dd4f91b1e8023167a98ad7 |
| Source note | uspto-grants-2014_11 |