HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 18612750, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Borane | HCID 6331 | — |
| Reactant | HCID 18612859 | HCID 18612859 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18612750 | HCID 18612750 | 77.4% |
Reaction Steps
A mixture of 1.6 g (3.57 mmol) of methyl 1-(methoxyacetyl)-4-(4-methoxybenzenesulfonyl)-2,3,4,5-tetrahydro-1H-[1,4]benzodiazepine-3-carboxylate and 32 ml of borane in tetrahydrofuran (1.0M) was refluxed under nitrogen overnight. Methanol was added and the solvent removed. To the residue was added 25 ml of CH2Cl2 and 25 ml of 2N HCl and the mixture stirred at room temperature for 1 hour. The organic layer was separated and washed with H2O and concentrated to dryness. The residue was triturated with ethyl acetate-hexane, cooled and filtered to give 1.2 g of white crystals, m.p. 86°-90° C.; Mass spectrum (ES) 435.4 (M+H). Anal. for C21H26N2O6S: Calc'd: C,58.1; H,6.0; N,6.5; Found: C.58.5; H,6.0: N,6.5.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06071903 |
| Source dataset | uspto-grants-2000_06 |
| ORD ID | ord-fe6351f8b93d4635a094165a6015e96e |
| Source note | uspto-grants-2000_06 |