HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,3-Dichloroacetone → 3-(4-Chloromethyl-thiazol-2-yl)-pyrrolidine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,3-Dichloroacetone | HCID 10793 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | Tert-butyl 3-carbamothioylpyrrolidine-1-carboxylate | HCID 5098610 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 3-(4-Chloromethyl-thiazol-2-yl)-pyrrolidine-1-carboxylic acid tert-butyl ester | HCID 57423800 | — |
Reaction Steps
To a solution of 3-thiocarbamoyl-pyrrolidine-1-carboxylic acid tert-butyl ester (1.06 g, 4.60 mmol) in acetone (25 mL) was added 1,3-dichloroacetone (0.76 g, 5.98 mmol), MgSO4 (0.83 g, 6.1 mmol) and MgCO3 (3.87 g, 4.6 mmol). The mixture was heated under reflux overnight, cooled and filtered through celite. The solvent was removed in vacuo and the residue was redissolved with EtOAc (20 mL). The resulting solution was washed successively with 5% NaHSO3, saturated NaHCO3, and brine. After drying (Na2SO4), the solvent was removed to afford the desired product which was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07638541B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-d1a3c93dad8b419ab4133fa5cc9682a1 |
| Source note | uspto-grants-2009_12 |