Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 178486892 | HCID 178486892 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178486891 | HCID 178486891 | — |
Reaction Steps
The procedure used in stage 4 of Example 216 is followed. In a 30 ml round-bottomed flask under an argon atmosphere, dissolve 140 mg of equimolecular mixture of 4-(5-fluoro-6-methoxy-1H-benzimidazol-2-yl)-9H-fluoren-9-one oxime (Z,E), obtained in the previous stage, in a mixture of 0.7 ml of ethanol, 0.7 ml of water and 0.7 ml of acetic acid. At room temperature, add 100 mg of zinc, in three stages, and, between each addition, stir for approximately one hour to two hours. After purification by flash chromatography on silica gel (40-63 μm), eluting with a mixture of dichloromethane and ammonia as a 7N solution in methanol (95/5 by volume), in this way we obtain 127 mg of 4-(5-fluoro-6-methoxy-1H -benzimidazol-2-yl)-9H-fluorene-9(R,S)-amine, in the form of a beige resin which is used as it is in the following stage, with the following characteristics:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07674795B2 |
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| Source dataset | uspto-grants-2010_03 |
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| ORD ID | ord-ced8ebabaf154be5aee417a6b13e2240 |
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| Source note | uspto-grants-2010_03 |
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