HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 86762525, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 2-Butenoic acid, 2-methyl- | HCID 6656 | — |
| Reactant | 2-Methylpentan-3-ol | HCID 11264 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86762525 | HCID 86762525 | 44% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
2-Methyl-pentan-3-ol (prepared as above in EXAMPLE I) (153 g), 2-methyl-but-2-enoic acid (100 g), toluene (200 mL), and PTSA (8 g) were charged into to 2-L reaction flask fitted with a Dean-Stark trap. The reaction mixture was heated to reflux at about 120° C. Water was removed. The reaction mixture was aged at reflux for about 13-14 hours till GC analysis showed completion of the reaction. The resulting reaction mixture was washed sequentially with sodium bicarbonate and brine, and further purified by fractional distillation to provide 2-methyl-but-2-enoic acid 1-ethyl-2-methyl-propyl ester (81 g) with a boiling point of 91° C. at 1.1 mmHg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772533B1 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-33a25f093d6f4e1da8682db1ece20fad |
| Source note | uspto-grants-2014_07 |