HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178507518, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 57885753 | HCID 57885753 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178507518 | HCID 178507518 | — |
Reaction Steps
To a solution of the above [4-({2-[2-(2-amino-phenylsulfanyl)-benzylamino]-5-nitro-pyrimidin-4-ylamino}-methyl)-cyclohexyl]-carbamic acid tert-butyl ester (35 mg, 0.06 mmol) in CH2Cl2 (10 mL) was added TFA (1.2 mL). The reaction mixture was stirred at room temperature for 2 h. The reaction mixture was then treated with saturated NaHCO3. During the work-up, some MeOH was added to solubilize the product in the organic phase. The organic phase was then dried over anhydrous Na2SO4 and concentrated in vacuo. The resulting residue was purified by silica gel preparative TLC using 10:1:0.1 CH2Cl2:MeOH:NH4OH as an eluent to afford 20 mg 70%) of the title compound as an off-white solid, m/z 477.9 (M−1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07601714B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-766ff3699c224e2bbe65f318ce34f867 |
| Source note | uspto-grants-2009_10 |