HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 15980787, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 3-Fluorobenzylic alcohol | HCID 68008 | — |
| Reactant | HCID 10018018 | HCID 10018018 | — |
| Catalyst | Sulfuric Acid | HCID 1118 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 15980787 | HCID 15980787 | 27% |
Reaction Steps
A solution of [5-(4-fluorophenylcarbamoyl)pyridin-2-ylsulfanyl]acetic acid (0.030 g, 0.10 mmole), 3-fluorobenzyl alcohol (0.10 mL, 1.0 mmol), and sulfuric acid (1 drop) in toluene (5 mL) was heated at reflux. After 2 h the reaction mixture was poured into ethyl acetate and washed with saturated sodium bicarbonate and dried over sodium sulfate. Removal of the solvents provided a solid. Purification by trituration using ethyl acetate/hexanes gave 0.011 g (27%) of the titled product as a white solid: 1H NMR (300 MHz, DMSO-d6) δ 10.36 (s 1H); 8.86 (m, 1H); 8.12 (m, 1H); 7.74 (m, 2H); 7.51 (m, 1H); 7.35 (m, 1H); 7.15 (m, 5H); 5.16 (m, 2H), 4.18 (m, 2H); MS (EI) m/z 413.05 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07151112B1 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-79bd3deb4819490da6d33874e720da67 |
| Source note | uspto-grants-2006_12 |