Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 1,3-Dioxolane-2-methanamine, N-methyl- | HCID 541754 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | HCID 12109531 | HCID 12109531 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 69148958 | HCID 69148958 | — |
Reaction Steps
1-Hydroxybenzotriazole (10.1 g) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (28.8 g) were added to a DMF (500 ml) suspension of 6-hydroxymethylthiazolo[3,2-a]benzimidazole-2-carboxylic acid (12.4 g), and the reaction mixture was stirred at room temperature for 1.5 hours. N-(1,3-Dioxolan-2-ylmethyl)-N-methylamine (17.1 ml) was added to the reaction mixture, and the resulting reaction mixture was stirred at the same temperature for 1 hour. After completion of the reaction, the reaction mixture was poured into 0.5 M sodium hydroxide aqueous solution (2 l). The insoluble matter was collected by filtration, washed with water and then with a mixed solvent of hexane and diethyl ether (mixing ratio; 3:1) and then dried by heating under a reduced pressure to obtain the title compound (8.62 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07250429B2 |
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| Source dataset | uspto-grants-2007_07 |
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| ORD ID | ord-714346f70d964eb8b952102dc9ed2614 |
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| Source note | uspto-grants-2007_07 |
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