HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 22999712, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | HCID 22999703 | HCID 22999703 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22999712 | HCID 22999712 | — |
Reaction Steps
To a string solution of 2-{[5-({[4-(tert-butyl)phenyl]sulfonyl}amino)-4-iodo-3-isoxazolyl]oxy}ethyl acetate (Preparation 23) (9.44 g) in dichloromethane was added pyridine (1.65 ml) followed by the slow addition of isobutylchloroforomate (2.41 ml) over 10 minutes. The reaction mixture was stirred at room temperature for one hour. The solvent was removed in vacuo to yield the crude material. This was purified using column chromatography (300 g silica, compound loaded with dichloromethane (15 ml)) using a gradient elution of hexane (100% to 75%) and ethyl acetate (0% to 25%) to yield the desired compound as a yellow oil (7.70 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06610518B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-49796d8d12364fea9e9ef1ab49fd8fb1 |
| Source note | uspto-grants-2003_08 |