HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86673825, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 68283314 | HCID 68283314 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86673825 | HCID 86673825 | — |
Reaction Steps
To a solution of (2S,5R)-5-hydroxymethyl-2-(3-trifluoromethoxy-phenylcarbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (390 mg, 0.97 mmol) in CH2Cl2 (3.5 mL) was added at 0° C. under nitrogen atmosphere Et3N (296 μl, 2.12 mmol) and mesylchloride (167 μl, 2.12 mmol) and the mixture was further stirred at RT for 3 h. CH2Cl2 and HCl 0.1N were added, the layers were separated and the aqueous one re-extracted with CH2Cl2. The crude organic extracts were washed with brine dried over Na2SO4, filtered and concentrated. The crude material was used without purification in the next step. MS (LC-MS): 383 [MH−Boc]+; tR (HPLC conditions b) 5.1 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09085555B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-e018cf41085542b7bc9cce92d3a6718d |
| Source note | uspto-grants-2015_07 |