HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 18423446, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 358625-61-3 | HCID 18423490 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18423446 | HCID 18423446 | 90.7% |
Reaction Steps
To a mixture of 0.06 g (2.5 mmol) of NaH in 5 mL of DMF at rt was added a solution of 0.1 g (0.39 mmol) of 1-t-butoxycarbonyl-4-(2-hydroxy-2-methyl-1-propyl)piperidine in 3 mL of DMF. After stirring for 20 min, 0.22 mL (3.5 mmol) of CH3I was added to the reaction mixture and the reaction mixture was stirred for 2 h. The reaction mixture was quenched with water and extracted with EtOAc. The combined organic fractions were washed with sat'd NaCl solution, dried over MgSO4, filtered and the filtrate was concentrated. The residue was purified by chromatography (silica, hexanes:ethyl acetate, 9:1) to give 0.096 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06455548B2 |
| Source dataset | uspto-grants-2002_09 |
| ORD ID | ord-a556bcf4eb524dec9f2bdb1ac6ce5fb4 |
| Source note | uspto-grants-2002_09 |