HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 72944854, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 90030421 | HCID 90030421 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | HCID 72944854 | HCID 72944854 | 9% |
Reaction Steps
Using similar reaction conditions as described in step-iii of example-1, N-(3-(3-(1-benzyl-1H-pyrazol-4-yl)-1-tosyl-1H-pyrrolo[2,3-b]pyridin-5-yl)phenyl)methanesulfonamide (60 mg, 0.1 mmol) was hydrolyzed by lithium hydroxide (9 mg, 0.2 mmol) in methanol/water/THF (1/1/1 ml) which afforded 4 mg (9% yield) after purification by preparative TLC (silicagel-1000 micron) using 5% methanol in chloroform as eluent. 1H NMR (DMSO-d6, 300 MHz): δ 8.46-8.45 (d, 1H), 8.34-8.33 (d, 1H), 8.14 (s, 1H), 7.9 (s, 1H), 7.62 (s, 1H), 7.54 (m, 1H), 7.5-7.43 (m, 2H), 7.37-7.33 (m, 2H), 7.3-7.27 (m, 3H), 5.4 (s, 2H), 3.0 (s, 3H). MS: m/z=443.6 (M+1), HPLC: 88.2%, Method A.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09353107B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-7868189da3f64be18b7ee01aebe57a85 |
| Source note | uspto-grants-2016_05 |