HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenesulfonyl chloride → HCID 11371056, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenesulfonyl chloride | HCID 7369 | — |
| Reactant | HCID 10058473 | HCID 10058473 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11371056 | HCID 11371056 | — |
Reaction Steps
A mixture of N,N-dimethyl-2-(6H-thieno[2,3-b]pyrrol-4-yl)ethylamine (0.2 mmol), benzenesulfonyl chloride (0.22 mmol) and KOt-Bu (0.22 mmol) in THF is shaken at ambient temperatures for 8 h and concentrated in vacuo. The resultant residue is dissolved in a mixture of DMSO, methanol and water and purified by preparative HPLC1 to afford the title product, [M+H] 335, retention time (RT) 1.42 min. 1Gilson Preparative HPLC conditions: Gilson Preparative HPLC system; YMC Pro C18, 20 mm×50 mm ID, 5 uM column; 2 mL injection; Solvent A: 0.02% TFA/water; Solvent B:0.02% TFA/acetonitrile; Gradient: Time 0: 95% A; 2 min: 95% A; 14 min: 10% A, 15 min: 10% A, 16 min: 95% A; Flow rate 22.5 mL/min; Detection: 254 nm DAD.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07220756B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-7f91ee9ca0c8427ca71053333fd2c1d2 |
| Source note | uspto-grants-2007_05 |