Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 19866454 | HCID 19866454 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19866472 | HCID 19866472 | 13.3% |
Reaction Steps
1.2 g (0.0027 mol) of 2-[3-(N-Morpholinyl)-n-propyl]- 4-(2-chlorophenyl)-9-methyl-6H-thieno[3,2-f][1,2,4]-triazolo[4,3-a][1,4]diazepine in 20 ml of anhydrous THF are added dropwise to a prepared suspension of 0.1 g (0.0027 mol) of lithium aluminium hydride in 20 ml of anhydrous THF at ambient temperature and the mixture is refluxed for one hour. 0.1 ml of water, 0.1 ml of 15% sodium hydroxide solution and 0.3 ml of water are added to the reaction mixture which is then stirred for 30 minutes and the precipitate obtained is suction filtered. The filtrate is concentrated by evaporation, taken up in methylene chloride, washed and dried and the solvent is removed. The residue is chromatographed on silica gel using methylene chloride/methanol 95:5 as eluant. 0.16 g (yield 13%) of the desired compound are obtained, m.p. 135°-138° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04900729 |
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| Source dataset | uspto-grants-1990_02 |
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| ORD ID | ord-731dd8bce99e4f1593fe2d44c6c49433 |
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| Source note | uspto-grants-1990_02 |
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