HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 59441878, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 59441746 | HCID 59441746 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59441878 | HCID 59441878 | 51% |
Reaction Steps
1-[3-(methyloxy)-4-nitrophenyl]-4-(methylsulfonyl)hexahydro-1H-1,4-diazepine (0.737g, 2.24 mmol) was suspended in 5 mL THF and 10 mL MeOH in a 100 mL round bottom flask. NiCl2-6H2O (159 mg, 0.672 mmol) was added followed by slow addition of NaBH4 (254 mg, 6.72 mmol). Reaction mixture was adsorbed onto SiO2 and purified via column chromatography to afford 2-(methyloxy)-4-[4-(methylsulfonyl)hexahydro-1H-1,4-diazepin-1-yl]aniline (340 mg, 51%) 1H NMR (400 MHz, DMSO-d6) δ ppm 1.82-1.94 (m, 2 H) 2.80 (s, 3 H) 3.17 (t, J=5.82 Hz, 2 H) 3.36-3.43 (m, 2 H) 3.49 (dd, J=10.68, 3.99 Hz, 4 H) 3.75 (br. s., 3 H) 4.01-4.15 (m, 2 H) 6.10-6.20 (m, 1 H) 6.26-6.35 (m, 1 H) 6.48-6.59 (m, 1 H). ESIMS (M+H)+301
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07981903B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-9190e9541440433f893a4fe268879a37 |
| Source note | uspto-grants-2011_07 |