Water → HCID 21393443, compound

HRID 461340Notes

Reaction equation

HRID 461340 reaction equation
[CH3:1][N:2]1[C:20](=O)[C:19](=O)[N:5]2[C:6]3[CH:18]=[CH:17][CH:16]=[N:15][C:7]=3[CH2:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[CH:4]2[CH2:3]1.[H-].[H-].[H-].[H-].[Li+].[Al+3].O>O1CCOCC1>[CH3:1][N:2]1[CH2:20][CH2:19][N:5]2[C:6]3[CH:18]=[CH:17][CH:16]=[N:15][C:7]=3[CH2:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[CH:4]2[CH2:3]1

Participants

5

Reactant 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 21393456HCID 21393456, compound

Product 1

HCID 21393443HCID 21393443, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
15 °C

Procedure

1.46 g (0.005 mol) 2-methyl-3,4-dioxo-1,2,3,4,10,14b-hexahydro-benzo[c]pyrazino[1,2-a]pyrido[2,3-f]azepine is added cautiously to a suspension of 0.4 g LiAlH4 in 25 ml dry dioxan under nitrogen at 25° C. The reaction mixture is boiled under reflux for 2 hours, after which it is cooled to 15° C. 5 ml water is then added, and the inorganic salts are filtered off and rinsed with dioxan. The filtrate is evaporated to dryness, giving a yellow oil. Melting point maleate salt: 163°-164° C (dec.).

Workup

  1. temperatureunder reflux for 2 hours
  2. filtrationthe inorganic salts are filtered off
  3. washrinsed with dioxan
  4. customThe filtrate is evaporated to dryness
  5. customgiving a yellow oil

Sources & evidence

ORD record
ord-4adcfe325f114931bb4d591890d574af
Source dataset
uspto-grants-1977_12
Patent number
US04062848

Reaction notes

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