HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 178505145, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 178511544 | HCID 178511544 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178505145 | HCID 178505145 | 49.1% |
Reaction Steps
To a solution of N4-[(trans-4-aminocyclohexyl)methyl]-5-nitro-N2-[2-(trifluoromethoxy)benzyl]-pyrimidine-2,4-diamine (50 mg, 0.11 mmol) were added methanesulfonyl chloride (18 μL, 0.23 mmol) and DIPEA (59 μL, 0.34 mmol) in CH2Cl2 (2 mL). The reaction mixture was stirred at room temperature for 15 min and diluted with CH2Cl2. The organic phase was then washed with 1M Na2CO3 and water. The organic phase was dried over Na2SO4 and concentrated. The resulting residue was purified by silica gel preparative TLC using 98:2 CH2Cl2:MeOH as an eluent to afford 28 mg (47%) of the title compound, m/z 517.7 [M−1]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07601714B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-fc39700b3d6a4605a7d72ccb6f65c393 |
| Source note | uspto-grants-2009_10 |