HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 10269594, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 22335621 | HCID 22335621 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 10269594 | HCID 10269594 | — |
Reaction Steps
Methyl 2-(4-fluorophenyl)-1-(4-methylsulphonylphenyl)-6,7-dihydro-5H-pyrrolizine-3-carboxylate (0.4 g, 0.96 mmol) is heated under reflux for 1 h in methanolic KOH (2 N, 9 ml, 1.01 g of KOH, 18 mmol). After cooling, water (20 ml) is added and the alkaline phase is rendered weakly acidic (pH 3) using HCl (conc. 25%). The deposited substance is extracted with ethyl acetate, and the ethyl acetate extract is dried using Na2SO4 sicc. and concentrated after filtering. After the removal of the solvent in vacuo, 0.4 g (75% GC) of residue remains. The CC purification is carried out on SiO2 using ethyl acetate as an eluent. The main fractions are concentrated in vacuo and the residue is recrystallized from diisopropyl ether:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06936632B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-5867c3c42b8542a8be050dc260a05d79 |
| Source note | uspto-grants-2005_08 |