Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86735879 | HCID 86735879 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20313862 | HCID 20313862 | 70.8% |
Reaction Steps
A solution of 3-[(1,3-benzodithiol-2-ylidene)amino]propanoic acid, ethyl ester (3.0g, prepared as described in Example 2) and sodium hydroxide (449 mg) in 120 ml of absolute ethanol is stirred at room temperature for 120 hours. The reaction mixture is concentrated in vacuo, and the resultant solid residue is washed with diethyl ether to remove unreacted starting material. The crude reaction product is dissolved in 50 ml of water, filtered through Celite, and the aqueous solution is then treated with 10% hydrochloric acid until the pH is 5. The resultant precipitate is collected by filtration and dried in vacuo at 60° C overnight. Recrystallization of the dried product from n-pentyl alcohol yields 1.9g of the title compound, melting point 203°-204° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04104467 |
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| Source dataset | uspto-grants-1978_08 |
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| ORD ID | ord-d04a5588ac9e483ca26f7215d352f0a8 |
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| Source note | uspto-grants-1978_08 |
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