HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 131726124, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Silane, tris(1-methylethyl)- | HCID 138754 | — |
| Reactant | HCID 58746870 | HCID 58746870 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 131726124 | HCID 131726124 | 18% |
Reaction Steps
A solution of 411-G of Example 4.11 (11 mg, 13 μmol) and triisopropylsilane (250 mL, 1.2 mmol) in trifluoroacetic acid (1.3 mL) was heated in a microwave at 170° C. for four minutes. The reaction mixture was diluted with toluene (5 mL) and evaporated. This was repeated until a residue appeared which was purified by preparative LCMS to yield the desired product (1.6 mg, 18%). 1H NMR (500 MHz, CD3OD): δ 7.46 (dd, J=8.8, 4.4 Hz, 1H), 7.32 (dd, J=9.3, 2.0 Hz, 1H), 7.19 (s, 1H), 7.14 (s, 1H), 7.08–7.04 (s, 1H), 5.44 (dd, J=8.8, 8.3 Hz, 1H), 4.03–3.98 (m, 1H), 3.98–3.84 (m, 2H), 3.79–3.70 (m, 1H), 3.52–3.42 (m, 1H), 3.41–3.39 (m, 1H), 3.33–3.27 (m, 1H), 3.13–3.01 (m, 3H); LCMS found for C20H20FN4O4S2 (M+H)+: m/z=463.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07141596B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-acf322cefa8a4033bc877586c4a87a80 |
| Source note | uspto-grants-2006_11 |