HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86590305, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 584218 | HCID 584218 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86590305 | HCID 86590305 | 82.7% |
Reaction Steps
To a stirred solution of 6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-9-ol (41.70 g, 0.255 mol) in CH2Cl2 (300 mL) at 0° C. was added triethylamine (72 mL, 0.517 mol) followed by methanesulfonyl chloride (30 mL, 0.388 mol). The resultant mixture was stirred at room temperature over night. The mixture was poured into water (200 mL) and the phases were separated. The organic phase was washed with brine (2×150 mL), dried (Na2SO4), and concentrated to give 50.87 g of crude methanesulfonic acid 6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-9-yl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07354934B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-063a3fabff6743c0ae460a5b627e6aaa |
| Source note | uspto-grants-2008_04 |