HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid monohydrate → HCID 59799080, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 57447748 | HCID 57447748 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 59799080 | HCID 59799080 | 79% |
Reaction Steps
Add p-toluensulfonic acid monohydrate (538 mg, 2.83 mmol) to a solution of 7-chloro-6-[2,2-dimethyl-3-(tetrahydro-pyran-2-yloxy)-propylamino]-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (1.190 g, 2.57 mmol) in methanol (80 mL). Stir the reaction at RT for 16 hr, concentrate, redissolve in EtOAc, wash with saturated aqueous sodium bicarbonate solution, brine, dry (sodium sulfate), concentrate and purify (silica gel chromatography, eluting with 1:4 EtOAc:hexanes) to give the title compound (750 mg, 79%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07981882B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-ab53cec2fab248658efc35c4eabbb810 |
| Source note | uspto-grants-2011_07 |