Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 70624874 | HCID 70624874 | — |
| Reactant | HCID 86736071 | HCID 86736071 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 70625700 | HCID 70625700 | — |
Reaction Steps
A solution of 6.8 g of (7RS,12aRS)-1,2,3,4,5,7,12,12a-octahydro-7-phenyl-1,4-diazepino[1,7-b]isoquinoline-3-carboxylic acid ethyl ester in toluene was added dropwise slowly into a stirred and boiling mixture of 200 ml of toluene and 21.6 ml of 70% disodium (2-methoxyethoxy)aluminium hydride in benzene. The reaction mixture was refluxed for a further 30 minutes, and cooled to 0°. The complex and remaining reducing agent was decomposed by the slow dropwise addition of 60 ml of a 20% sodium hydroxide solution. The organic phase was separated off, washed with 100 ml of a 20% sodium hydroxide solution, then washed three times with water, then dried with magnesium sulphate, and finally concentrated to dryness to give the title compound (M.P. of maleate from methanol/ether 184°-186°).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04120965 |
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| Source dataset | uspto-grants-1978_10 |
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| ORD ID | ord-0b43de09f6fe4c8d8fc03cfc8227845b |
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| Source note | uspto-grants-1978_10 |
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