HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isopropanol → HCID 135974500, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isopropanol | HCID 3776 | — |
| Reactant | 2-chloro-N,N-dimethylacetamide | HCID 75886 | — |
| Reactant | HCID 135741556 | HCID 135741556 | — |
| Product | HCID 135974500 | HCID 135974500 | 46% |
Reaction Steps
4-Hydroxy-3-methoxybenzenecarbothioamide (3.0 g, 16.37 mmol) (Example 35) and 2-chloro-N,N-dimethylacetamide were dissolved in isopropanol, and the mixture was heated at reflux for 12 h. The solvent was removed under reduced pressure. The residue was washed with water and extracted with ethyl acetate. The combined organic layers were dried over Na2SO4, filtered, and the solvent was removed in vacuo. Purification via silica gel flash chromatography (ethyl acetate/hexane (v/v)=1:4) yielded a solid (1.99 g, 46%). 1H NMR (400 MHz, CDCl3) δ 1.42 (d, 6H), 3.91 (s, 3H), 4.64 (septet, 1H), 5.95 (s, 1H), 6.0 (br, 1H), 6.91 (d, 1H), 7.36 (d, 1H), 7.53 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07592361B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-12ed633a09ba41c387558d1ad2356181 |
| Source note | uspto-grants-2009_09 |