HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → 3-iodo-N-methylbenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 3-Iodobenzoyl chloride | HCID 74378 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-iodo-N-methylbenzamide | HCID 3384366 | 26% |
Reaction Steps
To a cooled (0° C.) solution of 3-iodobenzoyl chloride (2.66 g; 10.0 mmol) in DCM (10 mL) was slowly added a 2 M solution of methylamine in THF (10 mL, 2.0 eq.). Upon completion of the addition, the ice bath was removed and the mixture was stirred overnight. All volatiles were removed in vacuo and the residue was treated with aq. NaHCO3 (25 mL) and subsequently extracted with ethyl acetate (3×15 mL). The combined organic layers were dried over MgSO4 and evaporated. The crude product was purified by column chromatography on silica gel to give the desired 3-iodo-N-methylbenzamide (0.67 g, 26% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08524724B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-2ccd5342a78a44c68040cb5a8f689b09 |
| Source note | uspto-grants-2013_09 |