Water → HCID 70636775, compound

HRID 1658720Notes

Reaction equation

HRID 1658720 reaction equation
[N:1]([CH:4]1[CH2:22][CH2:21][N:7]2[C:8]3[CH:20]=[CH:19][CH:18]=[CH:17][C:9]=3[CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:6]2[CH2:5]1)=[N+]=[N-].[H-].[H-].[H-].[H-].[Li+].[Al+3].O>CCOCC.CO.CC(C)=O>[NH2:1][CH:4]1[CH2:22][CH2:21][N:7]2[C:8]3[CH:20]=[CH:19][CH:18]=[CH:17][C:9]=3[CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:6]2[CH2:5]1

Participants

6

Reactant 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 86733598HCID 86733598, compound

Product 1

HCID 70636775HCID 70636775, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 21894497Aceton-methanolSolvent

Procedure

4 g of 2-azido-1,2,3,4,10,14b-hexahydro-pyridino[1,2-a]-dibenzo[c,f]-azepine (axial) is added to a suspension of 3 g of LiAlH4 in dry ether. The mixture obtained is heated for 1 hour, and after that cooled down. Then 12 ml of water are added to the mixture dropwise, whereby an inorganic precipitate is formed. The inorganic residue is removed by filtration after which the filtrate is evaporated to dryness. Obtained in this manner: 3.5 g (oil). Rf in methanol:acetone (9:1) = 0.28 (axial position).

Workup

  1. customThe mixture obtained
  2. temperatureis heated for 1 hour
  3. temperatureafter that cooled down
  4. customwhereby an inorganic precipitate is formed
  5. customThe inorganic residue is removed by filtration after which the filtrate
  6. customis evaporated to dryness
  7. customObtained in this manner

Sources & evidence

ORD record
ord-e5d035d8afbc496d944121abb6b75976
Source dataset
uspto-grants-1976_06
Patent number
US03966723

Reaction notes

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