Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Nitrobenzyl alcohol | HCID 11923 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Product | HCID 18983344 | HCID 18983344 | — |
Reaction Steps
Methanesulphonyl chloride (5.4 ml) was added dropwise to a stirred solution of 2-nitrobenzenemethanol (10.0 g) and triethylamine (10.1 ml) in 1,4-dioxane (10 ml) at 15°-25° C. After 30 min the mixture was filtered, washed with 1,4-dioxane (50 ml) and the filtrate added to a stirred mixture of 5-methylsalicylaldehyde (9.1 g) and potassium carbonate (9.9 g) in N,N-dimethylacetamide (50 ml). The mixture was stirred at 20° C. for 24 h, water (160 ml) was added and, after a further 1 h, the mixture was filtered. The filtrate was washed with water:1,4-dioxane (1:1; 50 ml) and water (150 ml) and dried at 40° C. in vacuo to give the title compound as a cream coloured solid (15.7 g) m.p. 124° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05332831 |
|---|
| Source dataset | uspto-grants-1994_07 |
|---|
| ORD ID | ord-9367ccf5077f4368aacc901d7d0f4180 |
|---|
| Source note | uspto-grants-1994_07 |
|---|