HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 59401155, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 59401096 | HCID 59401096 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59401155 | HCID 59401155 | 80.3% |
Reaction Steps
To a solution of hydroxy-(5-methyl-thiophen-2-yl)-acetic acid methyl ester (I265) (1.84 g, 9.89 mmol) in dry DCM, cooled at 0° C. under nitrogen atmosphere, N-ethyl-N-isopropylpropan-2-amine (2.54 mL, 14.8 mmol) and methanesulfonyl chloride (1.16 mL, 14.8 mmol) are added and the reaction is stirred at RT for 2 hours. DCM is added and the organic phase is washed with aq. NaHCO3, water and brine, dried over Na2SO4 and evaporated to obtain intermediate I268 as a dark brown oil (2.1 g, 80% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835682B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-55526f809b09481692e24c02781263b8 |
| Source note | uspto-grants-2014_09 |