Water → HCID 13520696, compound

HRID 1380856Notes

Reaction equation

HRID 1380856 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.O.[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

6

Reactant 4

HCID 962WaterHCID 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 lithium aluminum 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 iced water, 10% ammonium chloride solution is added and the precipitate formed is suction filtered. The filtrate is concentrated (to about 20 ml) in vacuo, the white precipitate obtained is suction filtered and washed with a little dioxan. Yield: 0.9 g. Mp: 162°-163° C.

Workup

  1. temperaturerefluxed for 3 hours
  2. additionis added
  3. customthe precipitate formed
  4. filtrationfiltered
  5. concentrationThe filtrate is concentrated (to about 20 ml) in vacuo
  6. customthe white precipitate obtained
  7. filtrationfiltered
  8. washwashed with a little dioxan

Sources & evidence

ORD record
ord-b6ae5c2cde2840a9a757fc68b3402fa5
Source dataset
uspto-grants-1986_04
Patent number
US04584293

Reaction notes

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