HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 118159540, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dimethylsulphamoyl chloride | HCID 83372 | — |
| Reactant | HCID 118159861 | HCID 118159861 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 118159540 | HCID 118159540 | — |
Reaction Steps
A solution of 7-(1-azetidin-3-yl-1H-pyrazol-3-yl)-6-(3-chlorobenzyl)-1-methyl-6H-pyrrolo[2,3-e][1,2,4]triazolo[4,3-a]pyridine bis(trifluoroacetate) salt (10.2 mg, 0.0158 mmol, prepared as in Example 156) in DCM (0.56 mL) was treated with triethylamine (11 μL, 0.079 mmol) and dimethylsulfamoyl chloride (2.5 μL, 0.024 mmol, Aldrich) and stirred for 35 minutes. Additional triethylamine (4.4 μL, 0.032 mmol) and dimethylsulfamoyl chloride (1.0 μL, 0.0093 mmol) were added. When the reaction was complete as determined by HPLC-MS, the product was purified via preparative HPLC-MS (Waters SunFire C18, eluting with a gradient of MeCN/H2O containing 0.1% TFA). Yield: (6.3 mg, 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09309246B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-cdb6302878464e8eb1cdce4f0d02ef95 |
| Source note | uspto-grants-2016_04 |