Ammonium Chloride → HCID 13520696, compound

HRID 1154636Notes

Reaction equation

HRID 1154636 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 ml of absolute dioxane was mixed with 2.2 gm (0.01 mol) of 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one, and the mixture was refluxed for 3 hours. Ammonium chloride solution (10%) was added while cooling with ice water, and the precipitate formed thereby was suction-filtered off. The filtrate was evaporated in vacuo to a volume of about 20 ml, and the resulting white precipitate was suction-filtered off and washed with a little dioxane.

Workup

  1. temperaturethe mixture was refluxed for 3 hours
  2. customthe precipitate formed
  3. filtrationthereby was suction-filtered off
  4. customThe filtrate was evaporated in vacuo to a volume of about 20 ml
  5. filtrationthe resulting white precipitate was suction-filtered off
  6. washwashed with a little dioxane

Sources & evidence

ORD record
ord-56293a4d6795493d90850919a3f55519
Source dataset
uspto-grants-1984_12
Patent number
US04490369

Reaction notes

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