Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 66679752 | HCID 66679752 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66680556 | HCID 66680556 | — |
Reaction Steps
172 ml (0.172 mol; 1.5 eq.) of 1N sodium hydroxide are added to a solution of 39.5 g (0.114 mol; 1 eq.) of (2,4-dioxo-1-p-tolyl-1,3-diazaspiro[4.5]dec-3-yl)acetic acid ethyl ester in 400 ml of THF. The reaction medium is stirred at room temperature for about 72 hours. The reaction medium is concentrated and 250 ml of ethyl acetate are added, followed by 400 ml of water. 100 ml of 1N NaOH are added and the aqueous solution is washed with 250 ml of ethyl acetate. The aqueous phase is concentrated and then acidified to pH 4 approximately with 170 ml of 1N acetic acid. The white precipitate is filtered off and then rinsed with water until the pH of the filtrates is approximately equal to 7, and dried in an oven under vacuum at 40° C. The product (2,4-dioxo-1-p-tolyl-1,3-diazaspiro[4.5]dec-3-yl)acetic acid is obtained in the form of a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08420681B2 |
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| Source dataset | uspto-grants-2013_04 |
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| ORD ID | ord-32559c43b1d041f9baa72d9c71be477a |
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| Source note | uspto-grants-2013_04 |
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