HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylacetamide → HCID 57901714, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylacetamide | HCID 31374 | — |
| Reactant | Thioacetamide | HCID 2723949 | — |
| Reactant | HCID 57901842 | HCID 57901842 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57901714 | HCID 57901714 | 11% |
Reaction Steps
A mixed solution of N-[2-(2-chloroacetyl)-1H-indol-7-yl]-N-methylthiophene-2-sulfonamide (570 mg), thioacetamide (0.20 g) and N,N-dimethylacetamide (15 ml) was stirred at 80° C. for 2 hr. The reaction solution was diluted with ethyl acetate, washed with water, aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was subjected to silica gel column chromatography (ethyl acetate:hexane=1:9-4:6), the obtained crude product was purified by preparative HPLC, and the obtained oil was crystallized from ethyl acetate-hexane to give the title compound (64 mg, yield 11%) as colorless needle crystals. melting point 161-162° C. MS:390 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957070B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-a2c971f5cdb14f2aa99f4aead328aa0a |
| Source note | uspto-grants-2015_02 |