Hydrochloric Acid → HCID 59021402, compound

HRID 970950Notes

Reaction equation

HRID 970950 reaction equation
CC12C3(C)[N:6]4[CH2:7][CH2:8][CH2:9][N:10]3[CH2:11][CH2:12][N:13]1[CH2:14][CH:15]([C:17]([O:19]C)=[O:18])[CH2:16][N:3]2[CH2:4][CH2:5]4.Cl>C(O)C>[NH:6]1[CH2:7][CH2:8][CH2:9][NH:10][CH2:11][CH2:12][NH:13][CH2:14][CH:15]([C:17]([OH:19])=[O:18])[CH2:16][NH:3][CH2:4][CH2:5]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 11243777HCID 11243777, compound

Product 1

HCID 59021402HCID 59021402, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
0 °C

Procedure

A solution of 0.50 g (1.62 mmol) of compound 3, prepared in example A, stage (b), in 20 ml of absolute ethanol is brought to reflux. 3 ml of a 35% aqueous hydrochloric acid solution are added in small amounts. Reflux is maintained for 48 hours. The mixture is cooled to 0° C. and the precipitate formed is filtered off and washed with ice-cold ethanol. The filtrate is evaporated and then the residue is taken up in the minimum amount of ethanol. The precipitate formed is filtered off and washed with ice-cold ethanol. Compound 6·3HCl is isolated in the form of a white powder (0.57 g, Yield =92%). Overall yield starting from the tetraamine: 87%.

Workup

  1. temperatureto reflux
  2. temperatureReflux
  3. temperatureis maintained for 48 hours
  4. customthe precipitate formed
  5. filtrationis filtered off
  6. washwashed with ice-cold ethanol
  7. customThe filtrate is evaporated
  8. customThe precipitate formed
  9. filtrationis filtered off
  10. washwashed with ice-cold ethanol
  11. customCompound 6·3HCl is isolated in the form of a white powder (0.57 g, Yield =92%)
  12. customOverall yield

Sources & evidence

ORD record
ord-13010f1648914c059db02cbb53331a10
Source dataset
uspto-grants-2007_12
Patent number
US07312327B2

Reaction notes

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