Water → HCID 70637164, compound

HRID 972946Notes

Reaction equation

HRID 972946 reaction equation
[H-].[H-].[H-].[H-].[Li+].[Al+3].[C:7]([CH:9]1[CH2:27][CH2:26][N:12]2[C:13]3[CH:25]=[CH:24][CH:23]=[CH:22][C:14]=3[CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[CH:11]2[CH2:10]1)#[N:8].O>CCOCC.C1COCC1>[NH2:8][CH2:7][CH:9]1[CH2:27][CH2:26][N:12]2[C:13]3[CH:25]=[CH:24][CH:23]=[CH:22][C:14]=3[CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[CH:11]2[CH2:10]1

Participants

6

Reactant 3

HCID 962WaterHCID 21226445Aluminium lithium hydride2×HCID 70637584HCID 70637584, compound

Product 1

HCID 70637164HCID 70637164, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 8028TetrahydrofuranSolvent

Procedure

To a suspension of 10 g LiAlH4 in 400 ml of dry ether a solution of 8 g of 2-cyano-1,2,3,4,10,14b-hexahydro-pyridino[ 1,2-a]-dibenzo[c,f]-azepine (axial) in 300 ml of THF is added. Then the mixture is refluxed for 30 minutes, whereupon it is cooled by means of ice. After that 40 ml of water are added to the mixture carefully so as to hydrolyse the excess of LiAlH4. The resulting precipitate is filtered off after which the filtrate is evaporated.

Workup

  1. additionis added
  2. temperatureThen the mixture is refluxed for 30 minutes, whereupon it
  3. temperatureis cooled by means of ice
  4. filtrationThe resulting precipitate is filtered off after which the filtrate
  5. customis evaporated

Sources & evidence

ORD record
ord-9dde9b8f59264878b0450ea324d83ecd
Source dataset
uspto-grants-1977_10
Patent number
US04054572

Reaction notes

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