HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68470799, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 12561769 | HCID 12561769 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 68470799 | HCID 68470799 | 95% |
Reaction Steps
Dissolve 7-methyl-1,4-dioxa-spiro[4.5]decane-8-carboxylic acid ethyl ester (R. R. Crenshaw, etc., J. Med. Chem., 1973, 16(7), 813-823) (14.09 g, 61.7 mmol) in MeOH (300 mL) and add 2M KOH (60 mL, 120 mmol, 2M in H2O). Stir the reaction for overnight at room temperature, then add 1N HCl until pH=3. Remove MeOH under reduced pressure and add water (200 mL). Extract the aqueous layer with ethyl acetate (3×400 mL). Combine the organic layers and dry with Na2SO4, filter and concentrate to give 11.74 g (95%) of the crude title compound as a white solid
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07713979B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-8960e1c5fb0b4389bb8bb1bbc7187fba |
| Source note | uspto-grants-2010_05 |