HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 2-Bromo-5-nitrobenzyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | (2-Bromo-5-nitrophenyl)methanol | HCID 18671373 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Bromo-5-nitrobenzyl methanesulfonate | HCID 86615392 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a solution of the (2-bromo-5-nitrophenyl)methanol from Step A (0.33 g, 1.42 mmol) in methylene chloride (20 ml) at 0° C., methanesulfonyl chloride (0.13 ml, 1.70 mmol) and triethylamine (0.3 ml, 2.1 mmol) were added. The solution was stirred at 0° C. for 1 h. The reaction was diluted with methylene chloride (30 ml). The solution was washed with water, brine, and dried over sodium sulfate. The title compound was obtained by flash column chromatography using 10:90 EtOAc/hexane as the eluant. 1H NMR (CDCl3, 500 MHz) δ 8.40 (d, J=2.5 Hz, 1H), 8.17 (dd, J=8.5, 3.0 Hz, 1H), 7.82 (d, J=8.5 Hz, 1H), 5.40 (s, 2H), 3.20 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08193365B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-c4585d77737748e99623dcbc2a01f2d1 |
| Source note | uspto-grants-2012_06 |