HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → 1-(1-Propyl)oxy-2,2,6,6-tetramethyl-4-trimethylsilyloxypiperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 4-trimethylsilyloxy-2,2,6,6-tetramethylpiperidine-N-oxide | HCID 58003880 | — |
| Product | 1-(1-Propyl)oxy-2,2,6,6-tetramethyl-4-trimethylsilyloxypiperidine | HCID 68315353 | — |
Reaction Steps
In another reaction vessel, 96.2 g (394 mmol) of 4-trimethylsilyloxy-2,2,6,6-tetramethylpiperidine-N-oxide was dissolved in 100 ml of dehydrated THF, and the Grignard reactant prepared was dropped at 0° C. After a reaction for 3 hours, the solution was concentrated by a rotary evaporator. 500 mL of water was added to the residue and an extraction was carried out using 500 mL in total of ethyl acetate, and the organic layer was concentrated by a rotary evaporator. The residue was purified by column chromatography (silica gel, hexane/ethyl acetate=20/1, volume ratio) to obtain 38.5 g of 1-(1-propyl)oxy-2,2,6,6-tetramethyl-4-trimethylsilyloxypiperidine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08912287B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-819e9ed3c969478a95ee910389950770 |
| Source note | uspto-grants-2014_12 |