HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 13477799, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 13477797 | HCID 13477797 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 13477799 | HCID 13477799 | 97.6% |
Reaction Steps
A mixture of 7.1 g (0.0286 mole) of 6H-indolo[2,1-c][1,4]benzodiazepin-12(11H)-one, the product of Example 1, 2.17 g (0.057 mole) of LAH and 100 ml of THF was refluxed for 5 hours under a nitrogen atmosphere. The reaction mixture was cooled to room temperature followed by the addition of 2.1 ml of water, 2.1 ml of 15% NaOH solution and 6.3 ml of water. The white solid obtained after 0.5 hour was filtered to give a light yellow filtrate which was concentrated in vacuo to give 6.54 g of off-white solid. Recrystallization from i-PrOH/EtOAc gave the title compound as a white solid, mp 176°-177° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04529724 |
| Source dataset | uspto-grants-1985_07 |
| ORD ID | ord-d3fde8a3045a4423908a1cad9d98510b |
| Source note | uspto-grants-1985_07 |