Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Solketal | HCID 7528 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 12151393 | HCID 12151393 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | HCID 23079405 | HCID 23079405 | 75.7% |
Reaction Steps
To 3 g of N,N-dimethylformamide, 300 mg of 5-chloro-3-ethoxymethylthio-1,2,4-thiadiazole and 188 mg of 2,2-dimethyl-1,3-dioxolane-4-methanol were dissolved, and added 62 mg of sodium hydride (60% in oil) at about 0° C., followed by stirring at about 0° C. for 30 minutes and standing at room tempareture for about 1 day. Then, to the reaction mixture, t-butylmethylether and saturated sodium chloride aqueous solution were added, and separeted to two layers. The organic layer was dried by anhydrous sodium salfate, and concentrated. The residue obtaind was subjected to column chromatography to obtain 330 mg of 5-(2,2-dimethyl-1,3-dioxolane-4-yl)methoxy-3-ethoxymethylthio-1,2,4-thiadiazole.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07342031B2 |
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| Source dataset | uspto-grants-2008_03 |
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| ORD ID | ord-95c6e5ec341842d7be030f1f1fb5f0ef |
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| Source note | uspto-grants-2008_03 |
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