Hydrochloric Acid → 5,11-Dihydro-11-[1-oxo-2-methyl-6-(4-methyl-1-piperazinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one dihydrochloride

HRID 4176Notes

Reaction equation

HRID 4176 reaction equation
[O:1]=[C:2]([N:16]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[C:20](=[O:27])[NH:19][C:18]2[CH:28]=[CH:29][CH:30]=[N:31][C:17]1=2)[CH:3]([CH3:15])[CH2:4][C:5]#[C:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]1.[ClH:32]>C(O)C>[ClH:32].[ClH:32].[O:1]=[C:2]([N:16]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[C:20](=[O:27])[NH:19][C:18]2[CH:28]=[CH:29][CH:30]=[N:31][C:17]1=2)[CH:3]([CH3:15])[CH2:4][C:5]#[C:6][CH2:7][N:8]1[CH2:9][CH2:10][N:11]([CH3:14])[CH2:12][CH2:13]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 139243965,11-Dihydro-11-[1-oxo-2-methyl-6-(4-methyl-1-piperazinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

Product 1

HCID 200649555,11-Dihydro-11-[1-oxo-2-methyl-6-(4-methyl-1-piperazinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one dihydrochloride

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

28 g (0.067 mol) of 5,11-dihydro-11-[1-oxo-2-methyl-6-(4-methyl-1-piperazinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one are suspended in 350 ml of absolute ethanol and 45 ml of ethereal hydrochloric acid are added with stirring at boiling temperature. A clear solution is obtained at first, which goes cloudy again after some time. A fine crystal slurry is precipitated which is cooled and suction filtered and then washed with 50 ml of absolute ethanol and 150 ml of acetone.

Workup

  1. customA clear solution is obtained at first, which
  2. customA fine crystal slurry is precipitated which
  3. temperatureis cooled
  4. filtrationsuction filtered
  5. washwashed with 50 ml of absolute ethanol and 150 ml of acetone

Sources & evidence

ORD record
ord-a11989da57094792a3813bfd266f2693
Source dataset
uspto-grants-1988_02
Patent number
US04724236

Reaction notes

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