HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 68670050, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 68671552 | HCID 68671552 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68670050 | HCID 68670050 | 35% |
Reaction Steps
To a stirring solution of crude diethyl 5-(aminomethyl)isophthalate in 30 mL of CH2Cl2 at 0° C. was added 1.2 mL of Et3N and 0.7 mL of MsCl. The ice bath was removed, and after 2 h at r.t. the solution was concentrated, and EtOAc and H2O were added. The organic layer was washed with brine, the aqueous layer was extracted with EtOAc, the combined extracts were dried over Na2SO4, filtered, and concentrated. Purification by flash silica gel chromatography (1% MeOH/CHCl3) provided 901 mg of diethyl 5-(methylsulfonamidomethyl)isophthalate as a pale yellow solid in 35% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299267B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-6d479df1c0144b438a5f1fc60fc7ae2c |
| Source note | uspto-grants-2012_10 |