Hydrochloric Acid → HCID 19698841, compound

HRID 862790Notes

Reaction equation

HRID 862790 reaction equation
[ClH:1].[CH2:2]([N:4](C(OC(C)(C)C)=O)[CH:5]([CH3:45])[CH2:6][CH2:7][N:8](C(OC(C)(C)C)=O)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][N:16](C(OC(C)(C)C)=O)[CH2:17][CH2:18][CH:19]([CH3:30])[N:20]([CH2:28][CH3:29])C(OC(C)(C)C)=O)[CH3:3]>CO>[ClH:1].[ClH:1].[ClH:1].[ClH:1].[CH2:28]([NH:20][CH:19]([CH3:30])[CH2:18][CH2:17][NH:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][NH:8][CH2:7][CH2:6][CH:5]([NH:4][CH2:2][CH3:3])[CH3:45])[CH3:29]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 19698835HCID 19698835, compound

Product 1

HCID 19698841HCID 19698841, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Add 1N HCl in methanol (50 ml) to 1,17-diethyl-2,16-dimethyl-1,5,13,17-tetra(t-butoxycarbonyl)-1,5,13,17-tetraazaheptadecane (3.9 g, 0.0054 mol) and stir overnight. Remove the solvent in vacuo and recrystallize the residue two times from methanol/acetonitrile (40/60, v/v) to yield 0.90 g of the title compound as a white solid (mp 249°-50° C.). Rf is 0.56 for TLC on silica gel developed with 40% conc. ammonia in methanol.

Workup

  1. customRemove the solvent in vacuo
  2. customrecrystallize the residue two times from methanol/acetonitrile (40/60

Sources & evidence

ORD record
ord-69152c3c96e047b7a05d0f9b833d94f7
Source dataset
uspto-grants-1998_02
Patent number
US05719193

Reaction notes

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