Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 11120579 | HCID 11120579 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 11023487 | HCID 11023487 | 97.4% |
Reaction Steps
1.5 g (4.78 mmoles) of the benzodiazepine derivative prepared in Step C are suspended in 60 ml of methanol, and to the suspension obtained, 4.64 g (57.3 mmoles) of concentrated hydrochloric acid are added, then, under cold water cooling, 2.07 g (54.8 mmoles) of sodium borohydride are added in portions. The suspension is stirred at 25° C. for 1 hour, then solid sodium carbonate is added to adjust the pH of the mixture to a value of about 8. The mixture is diluted with 60 ml of water, the product separated is filtered, washed 4 times using 5 ml of 50% aqueous methanol each time, and dried to obtain 1.47 g (97.4%) of the title compound. M.p.: 152°-154° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05807851 |
|---|
| Source dataset | uspto-grants-1998_09 |
|---|
| ORD ID | ord-bf1de563ccc74e1a98790c4f33a511c6 |
|---|
| Source note | uspto-grants-1998_09 |
|---|