Manganese(2+) dichloride → HCID 86750943, compound

HRID 976199Notes

Reaction equation

HRID 976199 reaction equation
[Cl-:1].[Mn+2:2].[Cl-:3].[CH2:4]([CH:22]1[CH2:36][NH:35][CH2:34][CH2:33][NH:32][CH2:31][CH2:30][NH:29][CH2:28][CH2:27][NH:26][CH2:25][CH2:24][NH:23]1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]>CO>[Cl:1][C:22]1([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:36][NH:35][CH2:34][CH2:33][NH:32][CH2:31][CH2:30][NH:29][CH2:28][CH2:27][NH:26][CH2:25][CH2:24][N:23]1[Cl:3].[Mn+2:2]

Participants

4

Reactant 2

HCID 10313134Manganese(2+) dichlorideHCID 18705601HCID 18705601, compound

Product 1

HCID 86750943HCID 86750943, compoundYield 75%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a refluxing solution of anhydrous manganese(II) chloride (0.18 g, 1.4 mmol) in anhydrous methanol (50 ml) was added 2-octadecyl-1,4,7,10,13-pentaazacyclopentadecane prepared as in example 28I (0.65 g, 1.4 mmol). The resulting solution was refluxed under a dry nitrogen atmosphere for 2 h and then stirred at room temperature overnight. The solvent was removed in vacuo, the oily residue redissolved in hot THF (20 ml) and filtered. The solution was concentrated and hot. ethyl ether was added with stirring to give 0.62 g (75% yield) of the product as a white solid: FAB mass spectrum (NBA) m/z (relative intensity) 556/558 [(M-Cl)+, 100/34]; Exact mass (M-Cl)+ : calcd., 557.3996; found, 557.4058 (C26H61N5MnCl).

Workup

  1. temperatureThe resulting solution was refluxed under a dry nitrogen atmosphere for 2 h
  2. customThe solvent was removed in vacuo
  3. dissolutionthe oily residue redissolved in hot THF (20 ml)
  4. filtrationfiltered
  5. concentrationThe solution was concentrated
  6. additionethyl ether was added
  7. stirringwith stirring

Sources & evidence

ORD record
ord-40c83c518f924d25827b5eeb8991b9e8
Source dataset
uspto-grants-1997_03
Patent number
US05610293

Reaction notes

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