HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 86652635, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | HCID 58229934 | HCID 58229934 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86652635 | HCID 86652635 | 14% |
Reaction Steps
To a solution of 8-[4-((R)-2,2,2-trifluoro-1-methyl-ethoxy)-phenyl]-1-oxa-8-aza-dispiro[2.2.4.2]dodecan-7-one (50 mg, 135 umol, obtained in example 252, Step 2) in chloroform was added tosic acid (26 mg, 135 umol) and the reaction mixture was stirred overnight at room temperature and then diluted with ethyl acetate. The organic layer was washed with brine, dried (Na2SO4), filtered and concentrated in vacuo to give a crude residue which was purified by flash column chromatography (grad 0% to 80% EtOAc in heptane) to yield the title compound as a white solid (7 mg, 14%). MS (m/e): 370.1 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08440710B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-4cbd39bcc5134553b6ab9b15d7453159 |
| Source note | uspto-grants-2013_05 |