HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → 1-bromo-N-[(1-formyl)propyl]-cyclopropane-1-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 1-bromo-N-[(1-hydroxymethyl)propyl]-cyclopropane-1-carboxamide | HCID 69426128 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | 1-bromo-N-[(1-formyl)propyl]-cyclopropane-1-carboxamide | HCID 18000860 | — |
Reaction Steps
2.23 ml of oxalyl chloride in 102 ml of methylene chloride is mixed drop by drop at −78° C. under nitrogen with 3.6 ml of dimethylsulfoxide in 41 ml of methylene chloride. Then, 5.43 g of amide alcohol 78 in 41 ml of methylene chloride and, after 15 minutes, 14.3 ml of triethylamine are added in drops at −78° C. After another 30 minutes, sodium chloride solution is added, extracted with methylene chloride, dried on sodium sulfate and concentrated by evaporation. The residue is chromatographed on silica gel with ethyl acetate/hexane, whereby 3.4 g of 1-bromo-N-[(1-formyl)propyl]-cyclopropane-1-carboxamide 79 is obtained as a yellow oil, which is converted into title compound 80 analogously to the reaction of amide 76.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06642218B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-53b5bb0caa2541aa8f7007530fd140fe |
| Source note | uspto-grants-2003_11 |