Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 178489836 | HCID 178489836 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178422922 | HCID 178422922 | 95.2% |
Reaction Steps
To a solution of trans-4-[(8-methoxy-7-methylquinazolin-2-yl)amino]cyclohexanol (16.7 g, 0.058 mol) in DMF (280 mL) was added NaSEt (11.9 g, 0.142 mol) in one portion at room temperature. The reaction mixture was stirred at 120° C. for 3 h. TLC (EtOAc) indicated the reaction was complete. DMF was removed in vacuo. The residue was taken up with water (200 mL), and the aqueous solution was adjusted to pH 6 with 1 N aq. HCl. The precipitate was filtered, washed with water (60 mL×2) and dried in vacuo to give the title compound (15.1 g, 95%) as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07998978B2 |
|---|
| Source dataset | uspto-grants-2011_08 |
|---|
| ORD ID | ord-9a890d1181a442758765362d81d5002c |
|---|
| Source note | uspto-grants-2011_08 |
|---|