HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dibutyltin dichloride → 3-[(4-Morpholin-4-yl-phenylamino)-methyl]1H-indole-6-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dibutyltin dichloride | HCID 12688 | — |
| Reactant | Phenylsilane | HCID 12752 | — |
| Reactant | Benzenamine, 4-(4-morpholinyl)- | HCID 75655 | — |
| Reactant | methyl 3-formyl-1H-indole-6-carboxylate | HCID 735867 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-[(4-Morpholin-4-yl-phenylamino)-methyl]1H-indole-6-carboxylic acid methyl ester | HCID 58930660 | 98% |
Reaction Steps
To a solution of 3-formyl-1H-indole-6-carboxylic acid methyl ester (500 mg, 2.46 mmol), 4-morpholinoaniline (482.3 mg, 2.71 mmol) and dibutyltin dichloride (76 mg, 0.25 mmol) in THF was added phenylsilane (334 μl, 2.71 mmol). The mixture was stirred at room temperature overnight under nitrogen, THF was evaporated off the mixture and the residue was purified by flash chromatography (hexane/EtOAc, 20/80) to afford the title compound 123 (881 mg, 98%). 1H-NMR (DMSO) δ: 8.00 (d, J=1.0 Hz, 1H), 7.70 (d, J=8.2 Hz, 1H); 7.58 (dd, J=8.4, 1.6 Hz, 1H); 7.52 (d, J=2.0 Hz, 1H); 6.70 (d, J=9.0 Hz, 2H); 6.59 (d, J=9.0 Hz, 2H); 5.48 (t, J=5.8 Hz, 1H); 4.31 (d, J=5.7 Hz, 2H); 3.83 (s, 3H); 3.68 (t, J=4.7 Hz, 4H); 2.86 (t, J=4.7 Hz, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08088805B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-a93867ec299d407ea2aeea786393e51a |
| Source note | uspto-grants-2012_01 |