HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoyl chloride → 3-(Methoxymethoxy)-6-neopentylpicolinonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | 5-(methoxymethoxy)-2-neopentylpyridine-N-oxide | HCID 67163656 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-(Methoxymethoxy)-6-neopentylpicolinonitrile | HCID 67165673 | 74% |
Reaction Steps
5-(Methoxymethoxy)-2-neopentylpyridine-N-oxide (11.5 g, 51 mmol) was dissolved in CH2Cl2 (50 mL) to which benzoyl chloride (12 ml, 102 mmol) and (trimethylsilyl)formonitrile (14 ml, 102 mmol) were added. The mixture was stirred under N2 4 h, quenched with saturated NaHCO3 (150 mL), and extracted with CH2Cl2 (3×100 mL). The combined organic layers were washed with saturated NaHCO3 (2×50 mL), dried (MgSO4), and evaporated to give the crude product as a brown oil, which was purified by ISCO (330 g SiO2, 0-40% EtOAc/Hexane) to give 3-(methoxymethoxy)-6-neopentylpicolinonitrile (8.8 g, 74% yield) as a clear oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08633315B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-0fde6bd1a2de4325bd043d788dbbfd14 |
| Source note | uspto-grants-2014_01 |