Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ammonium Carbonate | HCID 517111 | — |
| Reactant | HCID 18412288 | HCID 18412288 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 18412612 | HCID 18412612 | 78% |
Reaction Steps
1.5 g (3.0 mMol) of 1-methyl-2-[(4-cyanophenyl)methylthio]-benzimidazol-5-yl-carboxylic acid-N-phenyl-N-(2-ethoxycarbonylethyl)-amide were stirred in 80 ml of ethanol saturated with hydrogen chloride for 6.5 hours first at 0° C., then at room temperature, until no more starting material could be detected by thin layer chromatography. Then the solvent was distilled off at a maximum bath temperature of 30° C., the oily residue taken up in 80 ml of absolute ethanol and mixed with 1.0 g (10.5 mMol) of ammonium carbonate. After 18 hours the solvent was distilled off in vacuo and the crude product obtained was purified by flash chromatography (silica gel; methylene chloride/ethanol=19:1 to 10:1). Yield: 78% of theory of light beige solid, C28H29N5O3S (515.63) Rf value: 0.19 (silica gel; methylene chloride/ethanol=4:1) ##EQU92##
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06087380 |
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| Source dataset | uspto-grants-2000_07 |
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| ORD ID | ord-6a6a7a5b9fa542f39df39f6a381ba5be |
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| Source note | uspto-grants-2000_07 |
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