Water → HCID 70637164, compound

HRID 328137Notes

Reaction equation

HRID 328137 reaction equation
S(OC1CCN2C3C=CC=CC=3CC3C=CC=CC=3C2C1)(C1C=CC(C)=CC=1)(=O)=O.[C:31]([CH:33]1[CH2:51][CH2:50][N:36]2[C:37]3[CH:49]=[CH:48][CH:47]=[CH:46][C:38]=3[CH2:39][C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][C:41]=3[CH:35]2[CH2:34]1)#[N:32].O>CCOCC.C1COCC1>[NH2:32][CH2:31][CH:33]1[CH2:51][CH2:50][N:36]2[C:37]3[CH:49]=[CH:48][CH:47]=[CH:46][C:38]=3[CH2:39][C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][C:41]=3[CH:35]2[CH2:34]1

Participants

6

Reactant 3

HCID 962WaterHCID 70637584HCID 70637584, compoundHCID 86734600HCID 86734600, compound2×

Product 1

HCID 70637164HCID 70637164, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 8028TetrahydrofuranSolvent

Procedure

To a suspension of 10 g LiAlH 4 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 LiAlH 4. 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-519a16c179b34475b56f2ed6279884a3
Source dataset
uspto-grants-1977_04
Patent number
US04016161

Reaction notes

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