HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 59295975, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 59295944 | HCID 59295944 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 59295975 | HCID 59295975 | — |
Reaction Steps
tert-Butyl-4-[3,4-dichloro-2-(chlorosulfonyl)phenoxy]piperidine-1-carboxylate (0.80 g, 1.8 mmol) was dissolved in 7N ammonia in methanol and stirred at room temperature for 20 min. The solution was concentrated in vacuo and then azeotroped once with toluene. The residue was redissolved in dichloromethane:trifluoroacetic acid/1:1 (20 ml) and stirred at room temperature for 15 minutes. The solution was concentrated in vacuo, then partitioned between ethyl acetate and saturated aqueous sodium hydrogen carbonate solution. The aqueous was reextacted with ethyl acetate (4 times), and the combined organics dried over anhydrous potassium carbonate. Concentration in vacuo afforded the title compound as a white powder (0.54 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07709500B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-cfc3288bfb4a47b1b725a66aa703451b |
| Source note | uspto-grants-2010_05 |