HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 67218909, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Amino-2-methyl-1-propanol | HCID 11807 | — |
| Reactant | 5-Methyl-4-nitrothiophene-2-sulfonyl chloride | HCID 21498964 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 67218909 | HCID 67218909 | 58% |
Reaction Steps
To a stirred solution of 2-amino-2-methyl-1-propanol (1.11 g, 12.4 mmol) in dioxane (20 ml) was added at 0° C. (ice water bath) 5-methyl-4-nitrothiophene-2-sulfonyl chloride [CAS No. 61714-77-0] and triethylamine (0.63 ml, 4.56 mmol). The light yellow suspension was stirred at room temperature for 17 h, and evaporated. The crude product was further purified by column chromatography on silica gel (ethyl acetate/MeOH) and subsequent crystallization (ethyl acetate/heptane) to yield 5-methyl-4-nitro-thiophene-2-sulfonic acid (2-hydroxy-1,1-dimethyl-ethyl)-amide (0.71 g, 58%) as a light brown solid. MS (ISP) 293.0 [(M−H)−]; mp 126° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07361659B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-d26a6fd1b0a944549c9fbe71762a2cb2 |
| Source note | uspto-grants-2008_04 |