Hydrochloric Acid → HCID 19698848, compound

HRID 1031220Notes

Reaction equation

HRID 1031220 reaction equation
[ClH:1].[CH3:2][N:3](C(OC(C)(C)C)=O)[CH:4]([CH3:43])[CH2:5][CH2:6][N:7](C(OC(C)(C)C)=O)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][N:15](C(OC(C)(C)C)=O)[CH2:16][CH2:17][CH:18]([CH3:28])[N:19](C)[C:20](OC(C)(C)C)=O>CO>[ClH:1].[ClH:1].[ClH:1].[ClH:1].[CH3:20][NH:19][CH:18]([CH3:28])[CH2:17][CH2:16][NH:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][CH:4]([NH:3][CH3:2])[CH3:43]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 19698843HCID 19698843, compound

Product 1

HCID 19698848HCID 19698848, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Add lN HCl in methanol (50 ml) to 1,2,16,17-tetramethyl-1,5,13,17-tetra (t-butoxycarbonyl)-1,5,13,17-tetraazaheptadecane (3.8 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 0.74 g of the title compound as a white solid (mp 238°-9 ° C.). Rf is 0.31 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-3649a4bfbc1040818b70e69ff90015b0
Source dataset
uspto-grants-1992_04
Patent number
US05109024

Reaction notes

Loading…