Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Succinic Acid | HCID 1110 | — |
| Reactant | HCID 71656881 | HCID 71656881 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 71656972 | HCID 71656972 | 39% |
Reaction Steps
To 40.8 mg (0.056 mmol) of (5S)-4-(4,4-Difluorocyclohexyl)-3-{(S)-fluoro[4-(trifluoromethyl)phenyl]methyl}-2-{1-[5-(3-hydroxy-3-methylbutoxy)pyrimidin-2-yl]piperidin-4-yl}-7,7-dimethyl-5,6,7,8-tetrahydroquinolin-5-ol, which was prepared by a method similar to that of Reference Example 16, and 13.1 mg (0.11 mmol) of succinic acid, 0.08 ml of acetone and 0.008 ml of ultrapure water were added, and the reaction mixture was stirred at room temperature to obtain a homogeneous solution. A small amount of a seed crystal was added thereto, then 0.02 ml of acetone was added, and the reaction mixture was stirred for 30 minutes. The precipitated solid was obtained by filtration, washed with 0.4 ml of acetone and then dried under reduced pressure at 40° C. to provide 18.7 mg of the title compound as a white powder (yield: 39%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09321747B2 |
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| Source dataset | uspto-grants-2016_04 |
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| ORD ID | ord-faacc259d8ee4ea6a2cb5a33200e5fe4 |
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| Source note | uspto-grants-2016_04 |
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