Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 59479923 | HCID 59479923 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 25030663 | HCID 25030663 | 89.8% |
Reaction Steps
Adding water (20 mL), NaOH (0.14 g, 3.5 mmol) into a 100 mL round-bottom flask, stirring to dissolve, then adding 95% alcohol (20 mL), 4-((3,5,6-trimethylpyrazine-2-yl)methoxyl)benzoic acid ethyl ester (0.90 g, 3.0 mmol), stirring under room temperature to react for 4 hours, TLC [V(petroleum ether):V(ethyl acetate)=3:1 as developing agent] detecting shows that reaction is complete, (Rf of raw material=0.4, Rf of product=0), distilling out the alcohol under reduced pressure, adjusting pH of the reaction solution to 4-5 with 6.0M HCl while keeping the reaction solution cool to separate out solid, filtering, washing the solid with cool water for three times, processing with vacuum filtration, recrystallizing with anhydrous alcohol, drying under 70° C. for 8 hours to obtain 0.73 g white crystalloid of 4-((3,5,6-trimethylpyrazine-2-yl)methoxyl)benzoic acid, wherein a yield is 89.8%, m.p. 179-181° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08350033B2 |
|---|
| Source dataset | uspto-grants-2013_01 |
|---|
| ORD ID | ord-5ffe91b098404af8b27e99ba9c178ec5 |
|---|
| Source note | uspto-grants-2013_01 |
|---|