HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminium lithium hydride → 2-[1-Benzyl-3-(4-chloro-phenyl)-4,5,7,8-tetrahydro-1H-1,2,6-triaza-azulen-6-yl]-ethanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 59752513 | HCID 59752513 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-[1-Benzyl-3-(4-chloro-phenyl)-4,5,7,8-tetrahydro-1H-1,2,6-triaza-azulen-6-yl]-ethanol | HCID 59752680 | 33.5% |
Reaction Steps
To a solution of [1-benzyl-3-(4-chloro-phenyl)-4,5,7,8-tetrahydro-1H-1,2,6-triaza-azulen-6-yl]-acetic acid methyl ester (Example 170, 16 mg) in THF (1 mL) was added lithium aluminum hydride (100 mg). The mixture was stirred at RT for 16 h. The reaction was quenched by the addition of H2O (0.1 mL). Concentration and purification (SiO2, 2 M NH3 in MeOH/CH2Cl2) provided the title compound (5 mg). MS (ESI): exact mass calculated for C22H24ClN3O, 381.16; found, m/z 382.1 [M+H]+. 1H NMR (500 MHz, CDCl3): 7.50-7.20 (m, 7H), 7.04 (d, J=7.2 Hz, 1H), 5.29 (s, 2H), 3.07-3.04 (m, 2H), 2.89-2.77 (m, 10H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07579470B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-5c5e1a2dcc0c4cd6902d8166459b3b7c |
| Source note | uspto-grants-2009_08 |