HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium triacetoxyborohydride → 2-Oxo-1-[2-(4-{[(3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)methyl]amino)piperidin-1-yl)ethyl]-1,2-dihydroquinoxaline-6-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | 3-Oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazine-6-carbaldehyde | HCID 21873737 | — |
| Reactant | 1-[2-(4-Aminopiperidin-1-yl)ethyl]-2-oxo-1,2-dihydroquinoxaline-6-carbonitrile | HCID 66774135 | — |
| Product | 2-Oxo-1-[2-(4-{[(3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)methyl]amino)piperidin-1-yl)ethyl]-1,2-dihydroquinoxaline-6-carbonitrile | HCID 66774558 | 65.7% |
Reaction Steps
1-[2-(4-Aminopiperidin-1-yl)ethyl]-2-oxo-1,2-dihydroquinoxaline-6-carbonitrile (Intermediate 197, 0.125 g) was reacted with 3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazine-6-carbaldehyde (WO 2004/058144) (0.17 g) and NaBH(OAc)3 (0.27 g) as described for Example 107. The residue was purified by reverse phase HPLC with acetonitrile in water containing 0.1% TFA. Fractions containing product were concentrated to remove acetonitrile, neutralized with Na2CO3 solid, extracted with ethyl acetate, dried (Na2SO4), filtered and concentrated. The residue was suspended in diethyl ether and filtered to yield 127 mg of a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07875715B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-06f9effabb244d728f8d68ad0df2c869 |
| Source note | uspto-grants-2011_01 |