Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 34840-23-8 | HCID 6000134 | — |
| Reactant | HCID 68511467 | HCID 68511467 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86646931 | HCID 86646931 | 64.5% |
Reaction Steps
add 728 mg of dimethyl[(Z)-(methylsulphanyl)methylylidene]biscarbamate to a solution of 1 g of 4-[(2,6-dichlorobenzyl)oxy]benzene-1,2-diamine in a mixture of 60 cm3 of methanol and 212 mg of glacial acetic acid. The mixture is refluxed for 5.5 hours then concentrated under reduced pressure (0.2 kPa). The residue is taken up in 80 cm3 of a saturated aqueous solution in sodium hydrogen carbonate and the mixture obtained is extracted five times with 150 cm3 of ethyl acetate. The combined organic phases are dried over magnesium sulphate, filtered and evaporated under reduced pressure. The residue is taken up in 25 cm3 of acetonitrile, washed twice with 5 cm3 of acetonitrile, then dried under reduced pressure over sodium hydroxide. We obtain 834 mg of methyl {6-[(2,6-dichlorobenzyl)oxy]-1H-benzimidazol-2-yl}carbamate in the form of a white powder, which has the following characteristics:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08188078B2 |
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| Source dataset | uspto-grants-2012_05 |
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| ORD ID | ord-66d995a0ac7946028860f929da99793d |
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| Source note | uspto-grants-2012_05 |
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