Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phthalic Anhydride | HCID 6811 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 69004339 | HCID 69004339 | — |
| Solvent | P-Xylene | HCID 7809 | — |
| Product | HCID 68997739 | HCID 68997739 | 3.3% |
Reaction Steps
(E)-2-(4-{3-amino-4-[2-(1H-indazol-3-yl)vinyl]phenyl}piperazin-1-yl)ethanol (0.10 g, 0.28 mmol) obtained in Step 3 of Example 273 was dissolved in p-xylene (3.5 mL) and the solution was added with phthalic anhydride (49 mg, 0.33 mmol), triethylamine (0.02 mL, 0.14 mmol), molecular sieves 3A (0.10 g), followed by stirring at 140° C. for 25 hours. The solution was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The filtrate was reslurried with ethyl acetate to obtain Compound 299 (4.5 mg, 3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07605272B2 |
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| Source dataset | uspto-grants-2009_10 |
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| ORD ID | ord-63e1a346f808435db4b2dd4a5b5bda36 |
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| Source note | uspto-grants-2009_10 |
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