Manganese(2+) dichloride → HCID 86750562, compound

HRID 363384Notes

Reaction equation

HRID 363384 reaction equation
[C:1]1([CH2:7][CH:8]2[CH2:22][NH:21][CH2:20][CH2:19][NH:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13][NH:12][CH2:11][CH2:10][NH:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-:23].[Mn+2:24].[Cl-:25]>CO>[Cl:23][C:8]1([CH2:7][C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:22][NH:21][CH2:20][CH2:19][NH:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13][NH:12][CH2:11][CH2:10][N:9]1[Cl:25].[Mn+2:24]

Participants

4

Reactant 2

HCID 10313134Manganese(2+) dichlorideHCID 15521308HCID 15521308, compound

Product 1

HCID 86750562HCID 86750562, compoundYield 89%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 2-phenylmethyl-1,4,7,10,13-pentaazacyclopentadecane prepared as in Example 6D (1.5 g, 4.9 mmole) and anhydrous manganese(II) chloride (0.62 g, 4.9 mmole) in anhydrous methanol was refluxed under a dry nitrogen atmosphere overnight. The solution was filtered and the solvent removed in vacuo. The yellow gummy solid was purified by stirring vigorously in acetone to give 1.89 g (89% yield) of the product as a white solid: FAB mass spectrum (NBA) m/z (relative intensity) 395/397 [(M-Cl)+, 100/31]; Anal. calcd. for C17H31Cl2MnN5 : C, 47.34; H, 7.24; Cl, 16.44; N, 16.24. Found: C, 46.84; H, 7.51; Cl, 16.38; N, 15.86.

Workup

  1. temperaturewas refluxed under a dry nitrogen atmosphere overnight
  2. filtrationThe solution was filtered
  3. customthe solvent removed in vacuo
  4. customThe yellow gummy solid was purified

Sources & evidence

ORD record
ord-26724d4285bc431ca177414e6ab153b8
Source dataset
uspto-grants-1999_02
Patent number
US05874421

Reaction notes

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