HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 15952667, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 68687909 | HCID 68687909 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 15952667 | HCID 15952667 | 89% |
Reaction Steps
To a solution of methyl 4-{[3-{[(pyridin-3-ylmethyl)amino]carbonyl}-5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-yl]carbonyl}benzoate of Example 87 (0.315 g, 0.656 mmol) in methanol (4 mL) and water (2 mL) was added lithium hydroxide (31.4 mg, 1.31 mmol) and the reaction mixture heated to reflux for 1 hour. The cooled reaction mixture was diluted with water (20 mL) and washed with ethyl acetate (2×20 mL). The aqueous phase was then acidified to pH 4.5 by the addition of 2 M hydrochloric acid and the resulting milky suspension allowed to stand at 4° C. for 16 hours. The solid product was filtered, washed with water, and dried at 50° C. in vacuo overnight to afford the title compound (0.271 g, 89%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07678787B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-6c534065b294493f8009cdd4890e40b9 |
| Source note | uspto-grants-2010_03 |