HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-(Chloromethyl)pyridine hydrochloride → HCID 66987713, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-(Chloromethyl)pyridine hydrochloride | HCID 23394 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Tert-butyl 3-oxopiperazine-1-carboxylate | HCID 3157178 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66987713 | HCID 66987713 | — |
Reaction Steps
A mixture of 3-Oxo-piperazine-1-carboxylic acid tert-butyl ester (2.0 g, 9.99 mmol) and 3-Picolyl chloride hydrochloride (1.63 g, 9.99 mmol) in DMF (20 mL) is treated by 60% NaH in mineral oil (0.80 g, 19.98 mmol) at 0° C. After completion, the reaction mixture is quenched by H2O, EtOAc is added and the organic layer is washed with brine, dried over MgSO4 and evaporated in vacuo. Silica gel flash chromatography of the residue affords the title compound as a colorless oil; ES-MS: M+H=292.2et=4.15.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08053457B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-e298abe4381b4d23a9430ffcb9111389 |
| Source note | uspto-grants-2011_11 |