HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 69835993, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-(4-(Trifluoromethyl)phenyl)butane-1,3-dione | HCID 16640910 | — |
| Reactant | HCID 57098989 | HCID 57098989 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Trimethyl orthoformate | HCID 9005 | — |
| Product | HCID 69835993 | HCID 69835993 | — |
Reaction Steps
The title compound was prepared (as described above for the preparation of Example 2) from 57 mg (0.14 mmol) of Intermediate 60, 33 mg (0.14 mmol) of Intermediate 24, and 0.042 mL triethylamine in MeOH (1.5 mL) and trimethylorthoformate (0.5 mL) to yield 24 mg (28% yield) of Example 67 after silica gel chromatography (5%-15% MeOH in DCM): TLC (DCM/MeOH, 4/1): Rf=0.62; 1H NMR (DMSO-d6, 300 MHz) δ11.53 (d,1H, J=9.0), 7.97 (d, 2H, J=8.4), 7.89 (d, 2H, J=7.8), 7.73 (d, 2H, J=8.4), 7.46 (m, 3H), 7.97 (d, 2H, J=8.1), 6.79 (d, 2H, J=8.4), 5.62 (s, 1H), 4.25-4.19 (m, 1H), 3.90 (t, 2H, J=6.0), 3.21-3.15 (m, 1H), 2.58-2.83 (m, 5H), 1.98 (t, 2H, J=5.7), 1.72 (s, 3H), 1.11 (t, 3H, J=7.5); low resolution MS (ES+)m/e 607.18 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06498174B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-86d29139198a4f3f956c2cc7184c8ef3 |
| Source note | uspto-grants-2002_12 |