Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 3-Methylbutanal | HCID 11552 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | (4-Methanesulfonyl-phenyl)-[5-nitro-6-(piperidin-4-yloxy)-pyrimidin-4-yl]-amine | HCID 11257886 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 11190455 | HCID 11190455 | 36% |
Reaction Steps
Compound A2 (0.15 mmol, 60 mg), and 3-methyl-butyraldehyde (0.15 mmol, 13 mg) were dissolved in methanol (2 mL) and stirred for 5 minutes at room temperature. Then, sodium borohydride (0.18 mmol, 6.3 mg) was added at 0° C. The reaction was complete immediately upon addition of sodium borohydride. The mixture was quenched with saturated ammonium chloride solution (1 mL) followed by an extraction with dichloromethane. Removal of organic solvent in vacuo and purification by HPLC provided Compound A8 as a yellow solid (25 mg, 36%). 1H NMR (400 MHz, CDCl3) δ (ppm): 10.17 (s, 1H), 8.35 (s, 1H), 7.90 (d, 2H), 7.80 (d, 2H), 5.72 (s broad, 1H), 3.65 (m, 2H), 3.11 (m, 2H), 2.96 (m, 5H), 2.40 (m, 2H), 2.15 (m, 2H), 1.60 (m, 3H), 0.85 (d, 6H). LCMS (ESI), m/z 464.4 (M+H+, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08546429B2 |
|---|
| Source dataset | uspto-grants-2013_10 |
|---|
| ORD ID | ord-34bb1437d84943bf84b2b50cfde526d6 |
|---|
| Source note | uspto-grants-2013_10 |
|---|