HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 59464433, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 66911440 | HCID 66911440 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59464433 | HCID 59464433 | 105.2% |
Reaction Steps
To a solution of {4-[2-(2-tert-butoxycarbonylamino-phenylcarbamoyl)-vinyl]-phenyl}-hydroxy-acetic acid methyl ester (9.00 g, 21.1 mmol) and triethylamine (3.20 g, 31.6 mmol) in CH2Cl2 (135 mL) cooled to −5 degrees Celsius was added dropwise methanesulfonyl chloride (3.14 g, 27.4 mmol) under N2 atmosphere. The reaction was stirred at 0 degrees Celsius until the starting material had been consumed according to TLC (about 1 hour). The mixture was washed with water (90 mL) and brine (90 mL), dried with MgSO4, filtered, and evaporated in vacuo to obtain 11.2 g (quantitative yield) of light yellow crystal which was used without further purification. MS: calc'd 505 (MH+), exp 505 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07999000B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-47615dad85884f79b8bd0e649610982c |
| Source note | uspto-grants-2011_08 |