Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86603911 | HCID 86603911 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86603910 | HCID 86603910 | 84% |
Reaction Steps
Hydrochloric acid (1 ml of a 4.0 N solution in 1,4-dioxane, 4 mmol) was added, dropwise to a solution of di(tert-butyl) (1-(3-((4-((5-(2-((2-fluorophenyl)amino)-2-oxoethyl)-1,3-thiazol-2-yl)amino)-6-methoxyquinazolin-7-yl)oxy)propyl)piperidin-4-yl)methyl phosphate (assumed 379 mg, 0.49 mmol) in 1,4-dioxane (15 ml) upon which a light yellow solid precipitated from the reaction mixture. The resulting heterogeneous reaction mixture was stirred for a further 20 hours and the precipitate was filtered and washed with 1,4-dioxane (2×5 ml) then dried under high vacuum for 48 hours to furnish (1-(3-((4-((5-(2-((2-fluorophenyl)amino)-2-oxoethyl)-1,3-thiazol-2yl)amino)-6-methoxyquinazolin-7-yl)oxy)propyl)piperidin-4-yl)methyl dihydrogen phosphate bis-hydrochloride as a light yellow solid (302 mg, 84% yield):
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07407946B2 |
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| Source dataset | uspto-grants-2008_08 |
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| ORD ID | ord-88731302a63f4717bbb79d29b7a6cc6b |
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| Source note | uspto-grants-2008_08 |
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