Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanethiol | HCID 878 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 69878366 | HCID 69878366 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10131763 | HCID 10131763 | — |
Reaction Steps
2-Chloromethyl-1-phenylmethyl-1H-imidazo-[4,5-c]quinolin-4-amine hydrochloride (Example 28, prepared from 2.11 g of the alcohol) was added to a solution of methanethiol (1.33 g; 0.028 mol) and sodium methoxide (1.5 g; 0.028 mol) in methanol. The solid dissolved upon addition and a cream colored solid precipitated during addition. After stirring at room temperature for several hours the mixture was diluted with water. The solid was filtered from the mixture, washed with water, and dried. A crude yield of 2.3 g was obtained. The product was purified by silica gel flash chromatography (10% methanol in ethyl acetate eluent) and recrystallized from methanol/dichloromethane to give a cream colored solid, m.p. 217-219° C. Analysis: Calculated: C, 68.2; H, 5.4; N, 16.8. Found: C, 67.5; H, 5.3; N, 16.6.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06608201B2 |
|---|
| Source dataset | uspto-grants-2003_08 |
|---|
| ORD ID | ord-51a6744380204442a0060bb32516425a |
|---|
| Source note | uspto-grants-2003_08 |
|---|