HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nicotinic Acid → [((alpha-Nicotinoyloxyisobutoxy)carbonyl]aminomethyl}-1-Cyclohexane Acetic Acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nicotinic Acid | HCID 938 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 1-{[(alpha-Chloroisobutoxy)carbonyl]aminomethyl}-Cyclohexane Acetic Acid | HCID 22642007 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | [((alpha-Nicotinoyloxyisobutoxy)carbonyl]aminomethyl}-1-Cyclohexane Acetic Acid | HCID 11959211 | 14.5% |
Reaction Steps
A mixture of (93) (268 mg, 0.88 mmol), 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) (158 μL, 1.01 mmol), and nicotinic acid (637 mg, 5.2 mmol) in acetone was stirred at room temperature for 48 h. After filtration, the filtrate was concentrated in vacuo and the resulting residue was purified by reverse phase preparative HPLC to afford 50 mg (14%) of the title compound. 1H NMR (CD3OD, 400 MHz): δ 1.07 (d, J=6.8 Hz, 3H), 1.09 (d, J=6.8 Hz, 3H), 1.32-1.58 (m, 10H), 2.19 (m, 1H), 2.26 (s, 2H), 3.23 (m, 2H), 6.78 (d, J=4.8 Hz, 1H), 7.58 (m, 1H), 8.39 (d, J=6.4 Hz, 1H), 8.76 (d, J=4.4 Hz, 1H), 9.10 (s, 1H). MS (ESI) m/z 393.42 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367722B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-af2e402703e342fc93eddcfea7b85689 |
| Source note | uspto-grants-2013_02 |