Hydrochloric Acid → HCID 14346299, compound

HRID 970951Notes

Reaction equation

HRID 970951 reaction equation
CC12C3(C)[N:6]4[CH:7]([CH2:17][OH:18])[CH2:8][N:9]3[CH2:10][CH2:11][N:12]1[CH2:13][CH2:14][N:3]2[CH2:4][CH2:5]4.Cl>C(O)C>[NH:6]1[CH2:5][CH2:4][NH:3][CH2:14][CH2:13][NH:12][CH2:11][CH2:10][NH:9][CH2:8][CH:7]1[CH2:17][OH:18]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 69409774HCID 69409774, compound

Product 1

HCID 14346299HCID 14346299, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of 1.00 g (3.99 mmol) of compound 10 obtained in the preceding stage in 50 ml of absolute ethanol is brought to reflux. 10 ml of a 35% aqueous hydrochloric acid solution are added in small amounts. Reflux is maintained for 48 hours. After evaporation of the solvents, the residue is taken up in the minimum amount of ice-cold ethanol. The precipitate formed is filtered off and 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 11·4HCl is isolated in the form of a white powder (0.80 g, Yd =57%).

Workup

  1. temperatureto reflux
  2. temperatureReflux
  3. temperatureis maintained for 48 hours
  4. customAfter evaporation of the solvents
  5. customThe precipitate formed
  6. filtrationis filtered off
  7. washwashed with ice-cold methanol
  8. customThe filtrate is evaporated
  9. customThe precipitate formed
  10. filtrationis filtered off
  11. washwashed with ice-cold methanol
  12. customis isolated in the form of a white powder (0.80 g, Yd =57%)

Sources & evidence

ORD record
ord-fa24f97c50a243e4a4c6ef81117d8404
Source dataset
uspto-grants-2007_12
Patent number
US07312327B2

Reaction notes

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