Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | N-Methylformamide | HCID 31254 | — |
| Reactant | HCID 67708423 | HCID 67708423 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 67708522 | HCID 67708522 | — |
Reaction Steps
A mixture of 1.5 g (3 mMol) of tert.butyl 4'-[(2-n-propyl-4-methyl-6-(2-methyl-oxazol-4-yl)-benzimidazol-1-yl)-methyl]-biphenyl-2-carboxylate, 10 ml of 40% N-methylamine solution and 15 ml of N-methylformamide is heated for 10 hours to 200° C. in an autoclave. After cooling, the contents of the autoclave are stirred with about 40 ml of water, this suspension is adjusted to pH 6.5 with glacial acetic acid, then the crude product precipitated is suction filtered and dissolved in 1N sodium hydroxide solution. This solution is washed successively with 25 ml of acetic acid and diethylether, then adjusted to pH 6 with 20% citric acid. The product precipitated is suction filtered, washed with about 30 ml of water and dried, then triturated with diethylether and dried in a high vacuum.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05591762 |
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| Source dataset | uspto-grants-1997_01 |
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| ORD ID | ord-67c4ccbbf915463db595297d911309c4 |
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| Source note | uspto-grants-1997_01 |
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