HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalyl chloride → Tert-butyl 3-(3-(chlorocarbonyl)benzylthio)propanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 3-((3-Tert-butoxy-3-oxopropylthio)methyl)benzoic acid | HCID 66586713 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Tert-butyl 3-(3-(chlorocarbonyl)benzylthio)propanoate | HCID 86705208 | 99.6% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
Into a 100-mL round bottom flask, was placed a solution of 3-((3-tert-butoxy-3-oxopropylthio)methyl)benzoic acid 1.1c (3.00 g, 10.14 mmol, 1.00 equiv) in dichloromethane (50 mL). This was followed by dropwise addition of oxalyl dichloride (4.50 g, 35.43 mmol, 3.00 equiv) with stirring at 0° C. To this was added N,N-dimethylformamide (1 drop). The resulting solution was stirred for 1.5 h at room temperature. The resulting mixture was concentrated under vacuum to yield 3.18 g (99%) of tert-butyl 3-(3-(chlorocarbonyl)benzylthio)propanoate as red oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09289430B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-02dbe617499e44ba951870caaeae87fb |
| Source note | uspto-grants-2016_03 |