HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-(Chloromethyl)pyridine hydrochloride → 2-(4-Methoxy-benzensulfonyl)-2-methyl-3-pyridin-3-yl-propionic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-(Chloromethyl)pyridine hydrochloride | HCID 23394 | — |
| Reactant | 2-(4-Methoxy-benzenesulfonyl)propionic acid ethyl ester | HCID 20660503 | — |
| Catalyst | Benzyl triethylammonium chloride | HCID 66133 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | 2-(4-Methoxy-benzensulfonyl)-2-methyl-3-pyridin-3-yl-propionic acid ethyl ester | HCID 11046694 | — |
Reaction Steps
To a stirred solution of 2-(4-methoxy-benzenesulfonyl)propionic acid ethyl ester (2.7 gm, 10 mmol), 3-picolyl chloride hydrochloride (3.2 g, 20 mmol). and triethyl benzylammonium chloride (1 g) in methylene chloride (400 ml), 10 N NaOH (30 ml) was added. The reaction was continued at room temp for 48 hours. At the end, the organic layer was separated and washed well with water. The organic layer was dried, filtered and concentrated. The crude product obtained was purified by silica-gel column chromatography. The column was eluted with 50% ethyl acetate: hexane. 2-(4-Methoxy-benzensulfonyl)-2-methyl-3-pyridin-3-yl-propionic acid ethyl ester was isolated as brown oil. Yield 3.0 g, 82%; Brown oil; MS: 364 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06172057B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-1ec644bec65644d3a5444cfffb9e8aba |
| Source note | uspto-grants-2001_01 |