HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → Methanesulfonic acid 2-iodomethyl-5-methylphenyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Iodine | HCID 807 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Methanesulfonic acid 2-hydroxymethyl-5-methylphenyl ester | HCID 86638980 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methanesulfonic acid 2-iodomethyl-5-methylphenyl ester | HCID 86638982 | — |
Reaction Steps
To a solution of imidazole (4.5 g, 66.6 mmol) and PPh3 (17.4 g, 66.6 mmol) in DCM (180 mL) is slowly added over a period of 10 min of I2 (16.9 g, 66.6 mmol) and it is stirred at RT for 30 min. Then a solution of methanesulfonic acid 2-hydroxymethyl-5-methylphenyl ester (12.0 g, 55.5 mmol) in DCM (40 mL) is added drop wise and it is stirred at RT for 1 h. The reaction mixture is concentrated to about 70 mL. It is then filtered and washed with DCM. The filtrate is concentrated and purified to give the title compound as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08252820B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-078e7baf27854c9d8a5d867aaab1c13c |
| Source note | uspto-grants-2012_08 |