HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 72943270, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 90031121 | HCID 90031121 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | HCID 72943270 | HCID 72943270 | 28.2% |
Reaction Steps
Using similar reaction conditions as described in step-iii of example-1, N-(5-(3-(1-(2,5-difluorobenzyl)-3,5-dimethyl-1H-pyrazol-4-yl)-1-tosyl-1H-pyrrolo[2,3-b]pyridin-5-yl)-2-methoxy phenyl)methanesulfonamide (100 mg, 0.14 mmol) was hydrolyzed by lithium hydroxide (30.3 mg, 0.722 mmol), THF/Methanol/water (3/3/1 ml) to afford 13 mg (28.2% yield) of the titled compound after purification by column (SiO2-eluted by 2% MeOH in CHCl3). 1H NMR (CDCl3, 300 MHz): δ 9.37 (s, 1H), 8.54 (s, 1H), 7.84-7.78 (m, 2H), 7.37-7.35 (m, 1H), 7.02-6.99 (m, 1H), 6.95-6.85 (m, 1H), 6.80-6.60 (m, 2H), 5.29 (s, 2H), 3.94 (s, 3H), 2.99 (s, 3H), 2.25 (s, 3H), 2.17 (s, 3H). MS: m/z=538.1 (M+1), HPLC Purity: 91.44%, (Method: B).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09353107B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-886932326b7a4634a71f51f8f5e9c559 |
| Source note | uspto-grants-2016_05 |