Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | 2-Hydroxy-1,2,3-propanetricarboxylic acid hydrate (1:1) | HCID 22230 | — |
| Reactant | HCID 89907007 | HCID 89907007 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 118044993 | HCID 118044993 | — |
Reaction Steps
A mixture of (R)-2-(3-hydroxypyrrolidin-1-yl)-5-((4-(trifluoromethoxy)phenyl)carbamoyl)nicotinic acid ethyl ester (Stage 72.4, 3.20 g, 7.28 mmol) and LiOH in EtOH (18 mL)/water (6 mL) was stirred at 50° C. for 8 h. The solution was cooled to RT, acidified with citric acid monohydrate and resulting crystalline title compound was filtered and dried. m.p. 242-245° C., HPLC (Condition 4) tR=4.45 min, UPLC-MS (Condition 8) tR=0.80 min, m/z=412 [M+H]+; 1H-NMR (400 MHz, DMSO-d6) δ ppm 1.92 (br. s, 2H), 3.10 (d, J=12.12 Hz, 1H), 3.39 (br. s, 1H), 3.50-3.75 (m, 2H), 4.31 (br. s, 1H), 4.80-5.01 (m, 1H), 7.30 (d, J=8.60 Hz, 2H), 7.74-7.88 (m, 2H), 8.39 (d, J=2.35 Hz, 1H), 8.76 (d, J=2.35 Hz, 1H), 10.23 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09340537B2 |
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| Source dataset | uspto-grants-2016_05 |
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| ORD ID | ord-4eba0e3af8634b93906e9683368f128c |
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| Source note | uspto-grants-2016_05 |
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