Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Chloro-3-nitroquinoline | HCID 11275808 | — |
| Reactant | HCID 86619525 | HCID 86619525 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Dichloromethane ethylacetate | HCID 21226138 | — |
| Product | HCID 86619527 | HCID 86619527 | 89.9% |
Reaction Steps
tert-Butyl (2S)-2-amino-3-{[tert-butyl(dimethyl)silyl]oxy}propylcarbamate (3.43 g, 11.3 mmol) was dissolved in 110 mL of dry CH2Cl2. Triethylamine (3.14 mL, 22.6 mmol) and 4-chloro-3-nitroquinoline (2.35 g, 11.3 mmol) were then added and the reaction was stirred under N2 overnight. The reaction mixture was then treated with 100 mL of H2O and 100 mL of CH2Cl2. The layers were separated and the organic portion was washed successively with H2O and brine. The organic portion was dried over Na2SO4, filtered and concentrated under reduced pressure to give yellow solid. Chromatography (SiO2, 0-20% ethyl acetate/CH2Cl2) gave tert-butyl (2S)-3-{[tert-butyl(dimethyl)silyl]oxy}-2-[(3-nitroquinolin-4-yl)amino]propylcarbamate (4.84 g) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08034938B2 |
|---|
| Source dataset | uspto-grants-2011_10 |
|---|
| ORD ID | ord-bf3140ebedc84fb4a04db2d7d29409d7 |
|---|
| Source note | uspto-grants-2011_10 |
|---|