HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethanolamine → HCID 86607099, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethanolamine | HCID 8113 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Acetamido-4-methylthiazole-5-sulfonyl chloride | HCID 96951 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86607099 | HCID 86607099 | 58.2% |
Reaction Steps
To a stirred solution of diethanolamine (1.24 g, 11.8 mmol) in dioxane (20 ml) was added at 0° C. (ice water bath) commercially available 2-acetamido-4-methyl-thiazole-5-sulfonyl chloride (1.0 g, 3.93 mmol) and triethylamine (0.6 ml, 4.32 mmol). The light yellow suspension was stirred at room temperature for 17 h, and evaporated. The crude product was further purified by flash chromatography on silica gel (dichloromethane/MeOH) and subsequent crystallization (dichloromethane/MeOH/hexane) to yield 2-acetamido-4-methyl-thiazole-5-sulfonic acid bis-(2-hydroxy-ethyl)-amide (0.74 g, 58%) as a white solid. MS (ISP) 324.0 [(M+H)+]; mp 204° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07361659B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-5204fa72e49a41e4a5a05b0e6cd98bc2 |
| Source note | uspto-grants-2008_04 |