HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 57508889, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 57508888 | HCID 57508888 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Potassium bisulfate | HCID 516920 | — |
| Product | HCID 57508889 | HCID 57508889 | 132.3% |
Reaction Steps
A solution of 5,5-dimethyl-3-methylsulfanyl-4,5,6,7-tetrahydro-benzo[c]thiophene-1-carboxylic acid ethyl ester (458 mg, 1.61 mmol) and LiOH.H2O (696 mg, 16.6 mmol) in ethanol (5 mL), THF (3 mL) and water (0.6 mL) is stirred at rt overnight. The mixture is diluted with aq. KHSO4 and extracted with DCM. The organic extract is dried over Na2SO4, filtered and the solvent is removed in vacuo to give 5,5-dimethyl-3-methylsulfanyl-4,5,6,7-tetrahydro-benzo[c]thiophene-1-carboxylic acid (546 mg) as a beige solid; LC-MS: tR=1.00 min, [M+1]=257.6; 1H NMR (CDCl3): δ 2.98 (t, J=7.0 Hz, 2H), 2.49 (s, 3H), 2.34 (s, 2H), 1.55 (t, J=7.0 Hz, 2H), 0.98 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07723378B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-0b59de8ac3bf4ec3af0e6e0568b8a884 |
| Source note | uspto-grants-2010_05 |