HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 72944852, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 90031867 | HCID 90031867 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | HCID 72944852 | HCID 72944852 | 18% |
Reaction Steps
Using similar reaction conditions as described in step-iii of example-1, N-(3-(3-(1-(3-chlorobenzyl)-1H-pyrazol-4-yl)-1-tosyl-1H-pyrrolo[2,3-b]pyridin-5-yl)phenyl)methane sulfonamide (90 mg, 0.14 mmol) was hydrolyzed with lithium hydroxide (18 mg, 0.42 mmol) in THF/water/methanol (1/0.5/1 ml) mixture to afford 12 mg (18% yield) of the pure product after purification by preparative TLC (Silicagel-1000 micron) using 10% ethyl acetate in hexane as eluent. 1H NMR (DMSO-d6, 400 MHz): δ 11.83 (s, 1H), 9.85 (s, 1H), 8.48-8.47 (d, 1H), 8.43 (s, 1H), 8.346-8.342 (d, 1H), 7.90 (s, 1H), 7.80-7.79 (d, 1H), 7.51-7.25 (m, 8H), 5.40 (s, 2H), 3.06 (s, 3H). MS: m/z=478.2 (M+1), HPLC: 92.01% (method B).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09353107B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-dc3d909dede5467eae0a24c4c1cef6b1 |
| Source note | uspto-grants-2016_05 |