HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 22615022, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 2-Phenylethanethiol | HCID 78126 | — |
| Reactant | HCID 22615037 | HCID 22615037 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22615022 | HCID 22615022 | 97% |
Reaction Steps
To a solution of the compound in Example 11 (20 mg, 0.06 mmol) and phenethyl mercaptan (30 mg) in anhydrous CH2Cl2 (0.9 ml) was added trifluoroacetic acid (TFA, 0.2 ml). The mixture was stirred at room temperature for 2.5 hours. The solvent was removed under reduced pressure. The residue was purified over preparative TLC (CH2Cl2/MeOH=100/1) to give the desired compound (26 mg, 95%) as a colorless oil. FAB-MS: m/z 446 (MH+); 1H-NMR (CDCl3): δ 2.10 (2H, m), 2.32 (3H, s), 2.79-2.97 (6H, m), 3.54 (2H, s), 3.85 (2H, s), 3.90 (2H, s), 6.63 (1H, d, J=7.6 Hz), 7.09-7.30 (3H, m), 7.71 (1H, d, J=7.8 Hz), 8.55 (1H, d, J=2.0 Hz), 8.62 (1H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06376491B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-8fc0a6c5a7354f7c9b51c9bad2b5b1ec |
| Source note | uspto-grants-2002_04 |