Hydrochloric Acid → HCID 18940753, compound

HRID 356073Notes

Reaction equation

HRID 356073 reaction equation
[ClH:1].[CH2:2]([N:5](C(OC(C)(C)C)=O)[CH2:6][CH2:7][CH2:8][N:9](C(OC(C)(C)C)=O)[CH2:10][CH2:11][CH2:12][N:13]([CH2:21][CH2:22][CH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][NH:24]1)C(OC(C)(C)C)=O)[CH2:3][CH3:4]>CO>[ClH:1].[ClH:1].[ClH:1].[ClH:1].[CH2:2]([NH:5][CH2:6][CH2:7][CH2:8][NH:9][CH2:10][CH2:11][CH2:12][NH:13][CH2:21][CH2:22][CH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][NH:24]1)[CH2:3][CH3:4]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 18940747HCID 18940747, compound

Product 1

HCID 18940753HCID 18940753, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

30 ml of 3N methanolic hydrochloric acid are added to a solution of 2.07 g (3.54 mmol) of 1-propyl-9-[2-(2-piperidyl)-ethyl]-1,5,9-tri-BOC-1,5,9-triazanonane in 5 ml of methanol, and the reaction mixture is stirred at room temperature for 15 hours. The crystallisate is filtered off and the filtration residue is suspended in 15 ml of hot methanol. After cooling to room temperature, filtration, washing the crystallizate with ice-cold methanol and drying under a high vacuum at 100° C., the title compound is obtained, m.p. >270° C. 1H-NMR (D2O): δ =0.92(t,3H); 1.41-2.18(m,14H); 2.90-3.42(m,15H).

Workup

  1. filtrationThe crystallisate is filtered off
  2. temperatureAfter cooling to room temperature
  3. filtrationfiltration
  4. washwashing the crystallizate with ice-cold methanol
  5. customdrying under a high vacuum at 100° C.

Sources & evidence

ORD record
ord-e0faf224ccd44b0a90a051c73f4c3114
Source dataset
uspto-grants-1998_11
Patent number
US05834486

Reaction notes

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