Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 67421361 | HCID 67421361 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86635902 | HCID 86635902 | — |
Reaction Steps
To a solution of methyl-[4-(3,5,3″,5″-tetramethyl-3′,4′,5′,6′-tetrahydro-2′H-[2,2′;6′,2″]terpyridin-1′-yl)-butyl]-amine (168 mg, 0.440 mmol) in MeOH (1 mL) was added a saturated solution of HBr in MeOH (1 mL) according to General Procedure B. COMPOUND 81 was collected as a white solid (240 mg, 82%). 1H NMR (D2O) δ 1.19-1.31 (m, 4H), 1.46-1.56 (m, 2H), 1.65-1.70 (m, 1H), 1.90-1.95 (m, 1H), 2.11 (d, 2H, J=13.0 Hz), 2.22-2.27 (m, 2H), 2.50 (s, 6H), 2.55 (s, 6H), 2.57 (s, 3H), 2.75-2.81 (m, 2H), 4.53 (d, 2H, J=9.1 Hz), 8.26 (s, 2H), 8.51 (s, 2H); 13C NMR (D2O) δ 16.96, 17.56, 20.05, 22.43, 23.84, 32.65, 32.99, 48.80, 52.14, 57.55, 136.00, 137.42, 139.20, 150.10, 151.69; ES-MS nm/z 381 (M+H). Anal Calcd. For C24H36N4.3.0(HBr).2.1(H2O): C, 43.60; H, 6.59; N, 8.47; Br, 36.26. Found: C, 43.62; H, 6.38; N, 8.15; Br, 36.26.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07550484B2 |
|---|
| Source dataset | uspto-grants-2009_06 |
|---|
| ORD ID | ord-29df65332abb403490ba5c1fba970a53 |
|---|
| Source note | uspto-grants-2009_06 |
|---|