HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 90411586, compound → HCID 90411860, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 90411586 | HCID 90411586 | — |
| Solvent | Ammonia methanol | HCID 21705897 | — |
| Product | HCID 90411860 | HCID 90411860 | 67.1% |
Reaction Steps
A solution of 43 (2.0 g, 4.05 mmol) in 60 ml of 6 M NH3/MeOH was heated at 100° C. in a Parr bomb for 2 days. The reaction was cooled, concentrated and chromatographed on silica eluting, first, with ethyl acetate and, second, with 5% MeOH in ethyl acetate. Concentration of the product-containing fractions afforded 1.2 g (67%) of 44 as a white solid. 1H NMR (DMSO-d6): δ 7.39 (d, J=7 Hz, 1H), 6.94 (br s, 2H), 5.60 (d, J=7 Hz, 1H), 4.00 (m, 1H), 3.65 (m, 1H), 3.53 (m, 3H), 2.02 (m, 1H), 1.13 (d, J=6 Hz, 3H), 0.86 (s, 9H), 0.84 (s, 9H), 0.04 (s, 6H), −0.01 (s, 3H), −0.02 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169256B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-2ac051ae7bde405fa6fb13ab4d251034 |
| Source note | uspto-grants-2015_10 |