Hydrogen Bromide → HCID 178462464, compound

HRID 53527Notes

Reaction equation

HRID 53527 reaction equation
Br.[CH2:2]([N:4]1[C:10]2[N:11]=[CH:12][CH:13]=[CH:14][C:9]=2[C:8](=[O:15])[N:7]([CH3:16])[C:6]2[CH:17]=[CH:18][C:19]([O:21]C)=[N:20][C:5]1=2)[CH3:3]>C(O)(=O)C>[CH2:2]([N:4]1[C:10]2[N:11]=[CH:12][CH:13]=[CH:14][C:9]=2[C:8](=[O:15])[N:7]([CH3:16])[C:6]2[CH:17]=[CH:18][C:19]([OH:21])=[N:20][C:5]1=2)[CH3:3]

Participants

4

Reactant 2

HCID 260Hydrogen BromideHCID 463556Dipyridodiazepinone deriv. 36

Product 1

HCID 178462464HCID 178462464, compoundYield 28.1%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

Hydrobromic acid (48%, 2 ml) was added to a solution of 5,11-dihydro-11-ethyl-2-methoxy-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.3 g) in acetic acid (2 ml), and the resulting mixture was rapidly heated to reflux for 5 min. The reaction mixture was quenched with 10% sodium hydroxide (10 ml) and the product was extracted with ethyl acetate, dried (anhydrous magnesium sulfate) and concentrated to give a solid which was recrystallized from ethyl acetate to give 0.08 g of product, m.p. 215°-218° C.

Workup

  1. temperaturethe resulting mixture was rapidly heated
  2. temperatureto reflux for 5 min
  3. customThe reaction mixture was quenched with 10% sodium hydroxide (10 ml)
  4. extractionthe product was extracted with ethyl acetate
  5. dry with materialdried (anhydrous magnesium sulfate)
  6. concentrationconcentrated
  7. customto give a solid which
  8. customwas recrystallized from ethyl acetate

Sources & evidence

ORD record
ord-679032e71cfa4fefa416e543508140c0
Source dataset
uspto-grants-1997_04
Patent number
US05620974

Reaction notes

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