HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → 8-Methyl-2,3-dihydro-1,4-benzodioxine-6-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methyl 8-methyl-2,3-dihydro-1,4-benzodioxin-6-carboxylate | HCID 45122025 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 8-Methyl-2,3-dihydro-1,4-benzodioxine-6-carboxylic acid | HCID 45122024 | — |
Reaction Steps
A solution of 6.65 g (0.28 mol) LiOH in 100 mL water was metered into a solution of 33.60 g (0.16 mol) methyl 8-methyl-2,3-dihydro-1,4-benzodioxin-6-carboxylate in 200 mL THF and the reaction solution was stirred overnight at RT. To complete the reaction 150 mL 6 M NaOH were added and the mixture was stirred for a further 2 h at 50° C. The reaction mixture was evaporated down i.vac, the residue was combined with THF, acidified with conc. HCl while cooling with ice, the precipitate was filtered off, washed with 150 mL water and dried at 60° C. in the circulating air dryer.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07696195B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-5b61e9b4be5a420c8cd3368b8cc611f6 |
| Source note | uspto-grants-2010_04 |