Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 4-{[6-Chloro-2-(4-cyanoanilino)pyrimidin-4-yl]oxy}-3,5-dimethylbenzonitrile | HCID 50914946 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | GE-0012 | HCID 486367 | — |
Reaction Steps
4-[[6-chloro-2-[(4-cyanophenyl)amino]-4-pyrimidinyl]oxy]-3,5-dimethyl-benzonitrile (24 gm) was dissolved in aqueous ammonia (240 ml) and 1,4-dioxane (274 ml) at room temperature. The contents were heated to 120° C. and maintained for 12 hours at 120° C. To the reaction mass was added water (360 ml) and the reaction mass was slowly cooled to 50 to 60° C. The reaction mass was further cooled to 0 to 5° C. and stirred for 1 hour at 0 to 5° C., filtered. The wet solid obtained was dissolved in toluene (150 ml) under stirring. The separated solid was filtered and dried at 50° C. to obtain 10 gm of 4-[[6-amino-2-[(4-cyanophenyl)amino]-4-pyrimidinyl]oxy]-3,5-dimethylbenzonitrile.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08598341B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-1233d621d41b4be39f24cb0aa144ddf3 |
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| Source note | uspto-grants-2013_12 |
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