HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9902426, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Iodopropane | HCID 33643 | — |
| Reactant | 7,8-dimethoxy-1-phenyl-3,5-dihydro-4H-2,3-benzodiazepin-4-one | HCID 9860972 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 9902426 | HCID 9902426 | 72% |
Reaction Steps
Add dropwise under an inert atmosphere 400 μl of iodopropane to a solution of 200 mg (0.675 mmol) of 7,8-dimethoxy-1-phenyl-3,5-dihydro-4H-2,3-benzodiazepin-4-one VIaa and 121 mg (0.878 mmol) of K2CO3 in solution in 5 ml of DMF. After 72 hours at room temperature, add 30 ml of H2O and extract three times with 30 ml of Et2O. Dry the organic fractions on Na2SO4. Purify by chromatography (AcOEt 1/hexane 1). Yield: 72%. M: 48–52° C. 1H-NMR (300 MHz, CDCl3): d 0.83 (t, J=7.34, 3H, CH3), 1.65–1.72 (m, 2H, CH2CH3), 2.85–3.62 (m, 4H, CH2CH2CH3+5-CH2), 3.74 (s, 3H, OCH3), 3.98 (s, 3H, OCH3), 6.67 (s, 1H Ar), 6.89 (s, 1H Ar), 7.43–7.47 (m, 3H Ar), 7.65–7.68 (m, 2H Ar).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07250410B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-4f649cc348df4d9cb02272904c82c0e5 |
| Source note | uspto-grants-2007_07 |