Ammonium Chloride → HCID 13520696, compound

HRID 2290214Notes

Reaction equation

HRID 2290214 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 0.8 gm of lithium aluminium hydride in 100 of absolute dioxane is mixed with 2.2 gm (0.01 mol) of 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one and then refluxed for three hours. While the mixture is cooled with ice, 10% ammonium chloride solution is added, and the precipitate formed is subjected to suction filtration. The filtrate is concentrated in vacuo to a volume of about 20 ml, and the white precipitate is subjected to suction filtration and washed with a small amount of dioxane,

Workup

  1. temperaturerefluxed for three hours
  2. additionis added
  3. customthe precipitate formed
  4. filtrationis subjected to suction filtration
  5. concentrationThe filtrate is concentrated in vacuo to a volume of about 20 ml
  6. filtrationthe white precipitate is subjected to suction filtration
  7. washwashed with a small amount of dioxane

Sources & evidence

ORD record
ord-883e7d5488cc45fd9482895fa2e661b6
Source dataset
uspto-grants-1986_10
Patent number
US04616011

Reaction notes

Loading…