HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dibromobutane → HCID 178506372, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dibromobutane | HCID 8056 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 178511541 | HCID 178511541 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178506372 | HCID 178506372 | 43% |
Reaction Steps
To a solution of N4-[(trans-4-aminocyclohexyl)methyl]-N2-[2-(trifluoromethoxy)benzyl]-5-(trifluoromethyl)pyrimidine-2,4-diamine (100 mg, 0.22 mmol) in DMF (2 mL) were added 1,4-dibromobutane (140 mg, 0.65 mmol) and DIPEA (113 μL, 0.65 mmol). The reaction mixture was stirred at room temperature for 16 h and then heated at 65° C. for another 2 h. The reaction mixture was then diluted with EtOAc and washed with water (×4). The organic phase was dried over anhydrous Na2SO4 and concentrated in vacuo. The resulting residue was purified by silica gel preparative TLC using 10:1 CH2Cl2:MeOH as an eluent to afford 49 mg of the title compound as a while solid, m/z 518.6 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07601714B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-de6b0fc73fe64fcb88e7a33bb3087bbf |
| Source note | uspto-grants-2009_10 |