HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dimethoxyethane → HCID 66770720, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dimethoxyethane | HCID 8071 | — |
| Reactant | Sulfamide | HCID 82267 | — |
| Reactant | HCID 66770470 | HCID 66770470 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66770720 | HCID 66770720 | 88.4% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
180 mg of 5-(2,6-difluorophenyl)-7-fluoro-N-(piperidin-4-yl)-2-([2-(trimethylsilyl)ethoxy]methyl}-2H-pyrazolo[4,3-c]isoquinolin-3-amine, 2 ml of DME and 41 mg of sulphamide are mixed and microwave-heated at 150° C. for 1 h. The mixture is poured into water, extracted with AcOEt, washed with saturated NaCl solution, dried over MgSO4, filtered and concentrated under RP. The product is purified by flash chromatography on silica gel (15-40 μm), eluting with a DCM/methanol/aqueous ammonia mixture (95/05/0.5 by vol.), to give 183 mg of 4-{[5-(2,6-difluorophenyl)-7-fluoro-2-{[2-(trimethylsilyl)ethoxy]methyl}-2H-pyrazolo[4,3-c]isoquinolin-3-yl]amino}piperidine-1-sulphonamide (yellow solid). LC-MS-DAD-ELSD: 607=(M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461175B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-58617b9231d446e480e08f4b34a54127 |
| Source note | uspto-grants-2013_06 |