HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Anisoyl chloride → HCID 12069535, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Anisoyl chloride | HCID 7477 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| Reactant | tert-Butyl hydrogen (2-aminopyridin-3-yl)carbonimidate | HCID 13508831 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 12069535 | HCID 12069535 | 34.2% |
Reaction Steps
A solution of N3-(tert-butoxycarbonyl)-2,3-pyridinediamine (446 mg, 2.13 mmol) in tetrahydrofuran (7 mL) was treated with potassium hexamethyldisilazide (894 mg, 4.48 mmol). After 0.1 hr, the mixture was treated with p-anisoyl chloride (0.365 mL, 2.13 mmol). After 0.5 hr, the mixture was poured into aqueous ammonium chloride solution and ethyl acetate. The organic layer was washed three times with water, once with saturated sodium chloride solution, dried (magnesium sulfate), and filtered. Concentration in vacuo and purification of the residue by flash chromatography (silica gel, hexanes/ethyl acetate) yielded 250 mg (34%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313151B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-d51f43357eaa4ea198dce52b1c3ba98e |
| Source note | uspto-grants-2001_11 |