HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid monohydrate → Acetamide,n-[2-[4-[[3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl]amino]-5h-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl]-2-(methylsulfonyl)-,mono(4-methylbenzenesulfonate)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | N-{2-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-2-(methylsulfonyl)acetamide | HCID 57597166 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Acetamide,n-[2-[4-[[3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl]amino]-5h-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl]-2-(methylsulfonyl)-,mono(4-methylbenzenesulfonate) | HCID 76852991 | 76.9% |
Reaction Steps
To a solution of N-{2-[4-({3-chloro-4-[3-(trifluoromethyl)phenoxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-5-yl]ethyl}-2-(methylsulfonyl)acetamide (150 mg) in ethyl acetate (10 mL) was added 4-methylbenzenesulfonic acid monohydrate (55.4 mg) at room temperature. The mixture was stirred at room temperature for 20 hrs, and the solvent was evaporated under reduced pressure. The precipitated crystals were collected by filtration and washed with ethyl acetate and diisopropyl ether to give the title compound (150.3 mg) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178543B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-6e899469724a483ead3b7a3c9e49a8bf |
| Source note | uspto-grants-2012_05 |