HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 72943881, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 90031368 | HCID 90031368 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | HCID 72943881 | HCID 72943881 | 23% |
Reaction Steps
Using similar reaction conditions as described in step-iii of intermediate 1, 2-(4-(4-(3-(1-(3-fluorobenzyl)-3,5-dimethyl-1H-pyrazol-4-yl)-1-tosyl-1H-pyrrolo[2,3-b]pyridin-5-yl)phenyl) piperazin-1-yl)-N,N-dimethylethanamine (190 mg, 0.269 mmol) was hydrolyzed by lithium hydroxide (113 mg, 2.69 mmol), THF/Methanol/water (12/6/3 ml) to afford 34 mg (23% yield) of the titled compound. 1H NMR (CD3OD, 300 MHz): δ 8.432-8.426 (d, 1H), 7.835-7.829 (d, 1H), 7.512-7.475 (m, 2H), 7.367-7.324 (m, 1H), 7.069-6.968 (m, 3H), 6.878-6.845 (m, 1H), 5.349 (s, 2H), 3.68-3.48 (m, 2H), 3.162-3.12 (t, 2H), 2.967 (t, 1H), 2.82-2.715 (m, 8H), 2.206-2.166 (d, 6H), 1.923 (s, 1H). MS: m/z=552.2 (M+1); HPLC: 94.87% in method B.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09353107B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-1fd764d9e1c84f3b9c989f48676e9324 |
| Source note | uspto-grants-2016_05 |