Hydrochloric Acid → HCID 9813825, compound

HRID 970949Notes

Reaction equation

HRID 970949 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][CH3:20])=[O:18])[CH2:16][N:3]2[CH2:4][CH2:5]4.Cl>CO>[NH:6]1[CH2:7][CH2:8][CH2:9][NH:10][CH2:11][CH2:12][NH:13][CH2:14][CH:15]([C:17]([O:19][CH3:20])=[O:18])[CH2:16][NH:3][CH2:4][CH2:5]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 11243777HCID 11243777, compound

Product 1

HCID 9813825HCID 9813825, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
0 °C

Procedure

A solution of 5.00 g (16.2 mmol) of compound 3 prepared in the preceding stage in 50 ml of absolute methanol is brought to reflux. 30 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 then washed with ice-cold methanol. The filtrate is evaporated and then the residue is taken up in the minimum amount of methanol. The precipitate formed is filtered off and washed with ice-cold methanol. Compound 5·4HCl is isolated in the form of a white powder (4.55 g, Yield =76%). Overall yield starting from the tetraamine: 72%.

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 methanol
  7. customThe filtrate is evaporated
  8. customThe precipitate formed
  9. filtrationis filtered off
  10. washwashed with ice-cold methanol
  11. customis isolated in the form of a white powder (4.55 g, Yield =76%)
  12. customOverall yield

Sources & evidence

ORD record
ord-78ed072036f04e15adbdea1348f2113c
Source dataset
uspto-grants-2007_12
Patent number
US07312327B2

Reaction notes

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