HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyldimethylsilyl chloride → 7-bromo-N-((1S)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-methylethyl)-3-nitroquinolin-4-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Reactant | (2S)-2-[(7-bromo-3-nitroquinolin-4-yl)amino]propan-1-ol | HCID 67157472 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 7-bromo-N-((1S)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-methylethyl)-3-nitroquinolin-4-amine | HCID 67157627 | 100% |
Reaction Steps
A solution of (2S)-2-[(7-bromo-3-nitroquinolin-4-yl)amino]propan-1-ol (30.0 g, 92.0 mmol) dissolved in 100 mL of anhydrous pyridine was treated with tert-butyldimethylsilyl chloride (15.2 g, 101.2 mmol) and a catalytic amount of DMAP (112 mg, 0.92 mmol). After stirring overnight at ambient temperature under an atmosphere of N2, the reaction mixture was concentrated under reduced pressure. The resulting solid was partitioned between CH2Cl2 (500 mL) and H2O (500 mL). The layers were separated and the organic portion was concentrated under reduced pressure to give 40.5 g of 7-bromo-N-((1S)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-methylethyl)-3-nitroquinolin-4-amine as a yellow, crystalline solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08207162B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-513144b2d4ce473892066e6407a8eb9f |
| Source note | uspto-grants-2012_06 |