HuagongsheHuagongshe Chemistry Print Report · For research reference only
o-Toluenesulfonyl chloride → HCID 22099729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | o-Toluenesulfonyl chloride | HCID 8623 | — |
| Reactant | Methyl 2-[(4-ethoxy-4-oxobutyl)amino]benzoate | HCID 266836 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 22099729 | HCID 22099729 | 90.7% |
Reaction Steps
A mixture of 2.65 g of methyl 2-[(4-ethoxy-4-oxobutyl)amino]benzoate, 2.0 g of 2-methylphenylsulfonyl chloride and pyridine is heated on a steam bath for 16 hours. The mixture is concentrated under a vacuum (remove pyridine) and 1N HCl added. The mixture is extracted with dichloromethane and the extract washed with 1NHCl, H2O, 1M NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrons magnesium silicate and the filtrate evaporated to give 3.8 g of solid which is crystallized from ethanol to give crystals, m.p. 100°-102° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05849735 |
| Source dataset | uspto-grants-1998_12 |
| ORD ID | ord-8fef0a5ed1474e2fb06b85677cec9daf |
| Source note | uspto-grants-1998_12 |