HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 12082302, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 12082301 | HCID 12082301 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 12082302 | HCID 12082302 | 95.3% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
Methanesulfonic acid (11.6 g, 121 mmol) was added dropwise to a solution of the product from step B (10 g, 24.2 mmol) in CH2Cl2 (100 mL) over about 30 minutes. The reaction mixture was stirred for about 1 hour, then cooled to about 0° C., and then triethylamine (18.6 mL, 133.1 mmol) was added through an addition funnel. The mixture was allowed to warm to room temperature over about. 1 hour, diluted with additional CH2Cl2 and washed with saturated aqueous NaCl, dried over Na2SO4, filtered and concentrated in vacuo to afford the product as a white solid (7.2 g). 1H-NMR (CDCl3) δ: 2.51-2.72 (m, 4H), 3.35 (m, 2H), 3.49 (m, 2H), 4.03 (m, 1H), 4.25 (m, 1H), 7.08 (d, 2H), 7.51 (t, 1H), 8.37 (d, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06630487B2 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-a7d99eecc485476a91e6c2d77cebe3d5 |
| Source note | uspto-grants-2003_10 |