Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 178469990 | HCID 178469990 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178524818 | HCID 178524818 | 95.8% |
Reaction Steps
To a mixture of 1-[6-chloro-5-(4-chloro-benzenesulfonyl)-1H-benzoimidazol-2-yl]-1H-pyrazole-4-carboxylic acid ethyl ester (1.92 g, 4.13 mmol), THF (16 mL), and water (5 mL) was added LiOH.H2O (0.693 g, 16.5 mmol). The mixture was stirred for 18 h at 23° C. The solvent was evaporated, water (10 mL) was added and the mixture acidified with 1M HCl. The resulting precipitate was filtered and dried to yield the titled compound (1.73 g, 94%). MS (ESI/CI): mass calcd. for C17H10Cl2N4O4S, 436.0; m/z found, 437.0 [M+H]+. 1H NMR (500 MHz, DMSO-d6): 8.89 (s, 1H), 8.40 (s, 1H), 8.25 (s, 1H), 7.93-7.90 (m, 2H), 7.69-7.66 (m, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09073923B2 |
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| Source dataset | uspto-grants-2015_07 |
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| ORD ID | ord-972f7ea970a94b32a5796ea944b31d45 |
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| Source note | uspto-grants-2015_07 |
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