Hydrochloric Acid → HCID 14585900, compound

HRID 1291720Notes

Reaction equation

HRID 1291720 reaction equation
[CH2:1]([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][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][N:18](C(OC(C)(C)C)=O)[CH2:19][CH2:20][CH2:21][N:22]([CH2:30][CH2:31][CH2:32][CH3:33])C(OC(C)(C)C)=O)[CH2:2][CH2:3][CH3:4].Cl>CCO.CCOCC>[CH2:30]([NH:22][CH2:21][CH2:20][CH2:19][NH:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][NH:9][CH2:8][CH2:7][CH2:6][NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[CH2:31][CH2:32][CH3:33]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 23302093HCID 23302093, compound

Product 1

HCID 14585900HCID 14585900, compoundYield 98.4%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 3283Diethyl EtherSolvent

Procedure

Dissolve 1.32 gm (0.0017 mol) of the product of Step A of this example in 1.7 ml of EtOH, treat with 17 ml of 2N HCl in Et2O and stir the mixture overnight. Filter and wash the precipitate with Et2 O, recrystallize the washed material from isopropanol/water. Filter and dry the crystals (P2O5 at 79° C. at 0.1 mm) to yield 0.62 gm of the title compound, mp >300° C. Rf is 0.47 (silica gel plates eluted with 20% conc. NH3 /CH3OH).

Workup

  1. filtrationFilter
  2. washwash the precipitate with Et2 O
  3. customrecrystallize the washed material from isopropanol/water
  4. filtrationFilter
  5. dry with materialdry the crystals (P2O5 at 79° C. at 0.1 mm)

Sources & evidence

ORD record
ord-b526d169c8ba4c038b7cd7a2b5840dd8
Source dataset
uspto-grants-1998_05
Patent number
US05753714

Reaction notes

Loading…