HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 59406200, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N-BOC-ethylenediamine | HCID 187201 | — |
| Reactant | 5-Bromothiophene-2-sulfonyl chloride | HCID 2733924 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59406200 | HCID 59406200 | 96% |
Reaction Steps
To a stirred solution of commercially available 5-bromo-thiophene-2-sulfonyl chloride (1.0 g, 3.82 mmol) in THF (8 ml) was added at room temperature triethylamine (0.59 ml, 4.21 mmol), the mixture was cooled (ice-water) and a solution of commercially available N-BOC-ethylenediamine (1.82 ml, 11.5 mmol) in THF (8 ml) was added drop wise. The reaction mixture was stirred at room temperature for 16 h and evaporated. The crude product was further purified by flash chromatography (ethyl acetate/heptane) and subsequent crystallization from dichloromethane/hexane to yield the title compound (1.41 g, 96%) as a white solid. MS (ISN) 383.0 [(M−H)−], mp 106° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063048B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-b6b80e47277b44279bde0d2a240af73a |
| Source note | uspto-grants-2011_11 |