Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | 5-(4-Hydroxybenzyl)-3-triphenylmethylthiazolidine-2,4-dione | HCID 2818126 | — |
| Reactant | HCID 10852829 | HCID 10852829 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 10509356 | HCID 10509356 | — |
Reaction Steps
A procedure similar to that described in Preparation 4 was repeated, except that 0.5 g of 2-hydroxymethyl-3-(4-phenylbenzyl)imidazo[5,4-b]pyridine (prepared as described in Preparation 54), 0.738 g of 5-(4-hydroxy-benzyl)-3-triphenylmethylthiazolidine-2,4-dione, 0.43 ml of tributylphosphine, 0.4 g of 1,1'-(azodicarbonyl) dipiperidine and 20 ml of benzene were used, to give the title compound as a crude product. This crude product was purified by column chromatography through silica gel, using a gradient elution method, with mixtures of hexane and ethyl acetate in ratios ranging from 1:2 to 1:3 by volume as the eluent, to give 0.95 g of the title compound having Rf=0.44 (on silica gel thin layer chromatography using a 1:3 by volume mixture of hexane and ethyl acetate as the developing solvent).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06117893 |
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| Source dataset | uspto-grants-2000_09 |
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| ORD ID | ord-44452a45552b487ca97c7aeea23bf70c |
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| Source note | uspto-grants-2000_09 |
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