HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → 2-benzenesulfonyl-N-methylacetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Methyl phenylsulfonyl acetate | HCID 555619 | — |
| Product | 2-benzenesulfonyl-N-methylacetamide | HCID 9859184 | — |
Reaction Steps
The entire isolated, crude and moist phenylsulfonylacetic acid methyl ester (V) was transferred to a 2-L Erlenmeyer flask and dissolved in 1 L (11.7 mol) of 40% aqueous methylamine. The reaction temperature rose to 30° C. The mixture was allowed to cool to ambient temperature, and was maintained at this temperature for an additional hour, followed by cooling overnight in a refrigerator. The precipitate product (IV) was removed by filtration. The filter cake was washed with 3×300 mL of cold water. Drying the recovered white solid at 60° C. at 30 torr over potassium hydroxide flakes for 27 h yielded 402.7 g of the methylacetamide (IV), 97.3% purity by HPLC, mp 106-109° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06232471B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-05e4ae14cc2043c98a12cfd08cf1263f |
| Source note | uspto-grants-2001_05 |