Ammonium Chloride → HCID 13520696, compound

HRID 648959Notes

Reaction equation

HRID 648959 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[C:20]([O:21][CH3:22])=[CH:19][C:12]2[CH2:13][C:14](=O)[NH:15][CH:16]=[CH:17][C:11]=2[CH:10]=1.[Cl-].[NH4+]>O1CCOCC1>[CH3:22][O:21][C:20]1[C:9]([O:8][CH3:7])=[CH:10][C:11]2[CH2:17][CH2:16][NH:15][CH:14]=[CH:13][C:12]=2[CH:19]=1

Participants

5

Reactant 3

HCID 25517Ammonium ChlorideHCID 14823731,3-Dihydro-7,8-dimethoxy-2H-3-benzazepin-2-oneHCID 21226445Aluminium lithium hydride

Product 1

HCID 13520696HCID 13520696, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

A boiling suspension of of lithium aluminium hydride (0.8 g) in absolute dioxan (100 ml) is mixed with 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one (2.2 g, 0.01 mol) and then refluxed for 3 hours. While cooling with ice water, 10% ammonium chloride solution is added and the precipitate formed is suction filtered. The fitrate is evaporated in vacuo to a volume of about 20 ml, the white precipitate obtained is suction filtered and washed with a little dioxan.

Workup

  1. temperaturerefluxed for 3 hours
  2. additionis added
  3. customthe precipitate formed
  4. filtrationfiltered
  5. customThe fitrate is evaporated in vacuo to a volume of about 20 ml
  6. customthe white precipitate obtained
  7. filtrationfiltered
  8. washwashed with a little dioxan

Sources & evidence

ORD record
ord-ba15fbb4a2854e219dd038f801a7b44b
Source dataset
uspto-grants-1988_04
Patent number
US04737495

Reaction notes

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