Hydrogen Bromide → 5,11-Dihydro-11-[[[2-[2-[(dipropylamino)methyl]-piperidin-l-yl]ethy]amino]carbonyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one hydrobromide

HRID 2351441Notes

Reaction equation

HRID 2351441 reaction equation
[CH2:1]([N:4]([CH2:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][N:10]1[CH2:15][CH2:16][NH:17][C:18]([N:20]1[C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=2[C:24](=[O:31])[NH:23][C:22]2[CH:32]=[CH:33][CH:34]=[N:35][C:21]1=2)=[O:19])[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3].[BrH:36]>C(O)C>[BrH:36].[CH2:1]([N:4]([CH2:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][N:10]1[CH2:15][CH2:16][NH:17][C:18]([N:20]1[C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=2[C:24](=[O:31])[NH:23][C:22]2[CH:32]=[CH:33][CH:34]=[N:35][C:21]1=2)=[O:19])[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3]

Participants

4

Reactant 2

HCID 260Hydrogen BromideHCID 119357AF-DX-384

Product 1

HCID 679355455,11-Dihydro-11-[[[2-[2-[(dipropylamino)methyl]-piperidin-l-yl]ethy]amino]carbonyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one hydrobromide

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of 0.957 g (0.002 mol) of 5,11-dihydro-11-[[[2-[2-[(dipropylamino)methyl]-piperidin-l-yl]ethyl]amino]carbonyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one in 20 ml of ethanol was combined with 0.135 ml of a 45% aqueous hydrobromic acid solution (0.002 mol). The colourless salt mentioned above slowly crystallised out of the mixture and after being left to stand for 3 hours it was suction filtered, washed thoroughly three times with 3 ml of anhydrous ethanol and finally dried at 50° C. in a circulating air dryer.

Workup

  1. customabove slowly crystallised out of the mixture
  2. waitafter being left
  3. filtrationfiltered
  4. washwashed thoroughly three times with 3 ml of anhydrous ethanol
  5. customfinally dried at 50° C. in a circulating air dryer

Sources & evidence

ORD record
ord-08ae2f68e9214de2a09c5b94c1bf956b
Source dataset
uspto-grants-1989_10
Patent number
US04873236

Reaction notes

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