HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 53439675, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 13023786 | HCID 13023786 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 53439675 | HCID 53439675 | 96% |
Reaction Steps
To a cold mixture of 3,3-dimethyl-1-nitro-butan-2-ol (7.35 g, 50.0 mmol), and triethylamine (17.4 mL, 125 mmol) in dichloromethane (70 mL) at −78° C. was added MsCl (4.64 mL, 60 mmol) dropwise; the mixture was stirred for 2 hours at −78° C. to room temperature. Then solvents were removed, the residue was partitioned between EtOAc and diluted HCl aqueous solution, the EtOAc phase was washed with saturated NaCl aqueous solution, then dried over anhydrous sodium sulfate, filtered, concentrated, to give an oil, the title compound (6.2 g); The title product, 1H NMR (200 MHz, CDCl3): δ (ppm)=7.25 (d, 1H, J=13.4 Hz), 6.88 (d, 1H, J=13.4 Hz), 1.16 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07696223B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-1e41ce8926e14258b5b6ed1c9a639d7d |
| Source note | uspto-grants-2010_04 |