HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Hordenine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | 4-(2-Bromoethyl)phenol | HCID 84221 | — |
| Product | Hordenine | HCID 68313 | 92% |
Reaction Steps
To 250 mg of 4-hydroxyphenethyl bromide in a round-bottomed flask, a 10 M excess of methylamine (6.22 mL of 2M in MeOH) was added and the solution was stirred at r.t. overnight. After filtration, the solvent was evaporated and gave the product in crystalline form in 92% yield, 0.23 g, light yellow. m.p.: 73-76° C. TLC (EtAc:MeOH, 9:1 v/v): RF=0.1. 1H NMR, δ: 9.43 (s, 1H), 7.12 (d, 2H), 6.70 (d, 2H), 2.74 (m, 4H), 2.30 (s, 6H). 13C NMR, δ: 167.5, 134.3, 130.2, 115.6, 60.6, 45.9, 32.4. Anal. calcd for C10H15NO: C, 72.69; H, 9.15; N, 8.48%. Found; C, 72.60; H, 9.30; N, 8.40%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08349898B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-26d15eaa88864d118bb96eff8476c9bf |
| Source note | uspto-grants-2013_01 |