HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 87191905, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 87191894 | HCID 87191894 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 87191905 | HCID 87191905 | — |
Reaction Steps
To a solution of Example 33 (0.04 g, 0.095 mmol) in 2 mL anhydrous THF was added diisopropylethylamine (0.07 mL, 0.38 mmol) followed by methanesulfonyl chloride (0.009 mL, 0.114 mmol). The resulting solution was stirred at room temperature for 2.5 hours. The reaction mixture was diluted with ethyl acetate and washed with water, brine, dried over magnesium sulfate, filtered, and concentrated to give the title compound as an off-white solid. 1H NMR (300 MHz, DMSO-d6) ppm 1.16-1.35 (m, 1H) 1.38-1.61 (m, 3H) 1.93-2.10 (m, 3H) 2.90-3.04 (m, 2H) 3.52 (d, J=12.21 Hz, 2H) 3.84 (s, 1H) 6.82-7.00 (m, 3H) 7.21 (dd, J=7.80, 5.09 Hz, 1H) 8.14 (d, J=3.05 Hz, 1H) 8.24-8.37 (m, 2H) 12.16 (s, 1H). MS (ESI+) m/z 406.0 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08435980B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-5f49150ffa5342fdb9afd94fe20a0685 |
| Source note | uspto-grants-2013_05 |