Manganese(2+) dichloride → HCID 86750560, compound

HRID 363380Notes

Reaction equation

HRID 363380 reaction equation
[CH3:1][CH:2]([CH3:19])[CH2:3][CH:4]1[CH2:18][NH:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][NH:8][CH2:7][CH2:6][NH:5]1.[Cl-:20].[Mn+2:21].[Cl-:22]>CO>[Cl:20][C:4]1([CH2:3][CH:2]([CH3:19])[CH3:1])[CH2:18][NH:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][NH:8][CH2:7][CH2:6][N:5]1[Cl:22].[Mn+2:21]

Participants

4

Reactant 2

HCID 10313134Manganese(2+) dichlorideHCID 10453397HCID 10453397, compound

Product 1

HCID 86750560HCID 86750560, compoundYield 48%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 2-(2-methylpropyl)-1,4,7,10,13-pentaazacyclopentadecane prepared as in Example 5D (0.66 g, 2.4 mmole) and anhydrous manganese(II) chloride (0.31 g, 2.4 mmole) in anhydrous methanol (40 ml) was refluxed under a dry nitrogen atmosphere overnight. The solution was filtered and the solvent removed in vacuo. The resulting yellow solid was recrystallized from THF-ethyl ether to give 0.46 g (48% yield) of the product as an off-white solid: FAB mass spectrum (NBA) m/z (relative intensity) 396 (M+, 1), 361/363 [(M-Cl)+ 84/26], 272 [(M-MnCl2 +H) + 100]. Anal. Calcd. for C14H33Cl2MnN5 : C, 42.33; H, 8.37; N, 17.63. Found: C, 41.90; H, 8.22; N, 17.30.

Workup

  1. temperaturewas refluxed under a dry nitrogen atmosphere overnight
  2. filtrationThe solution was filtered
  3. customthe solvent removed in vacuo
  4. customThe resulting yellow solid was recrystallized from THF-ethyl ether

Sources & evidence

ORD record
ord-12fdf74cae6d41489a31b6bbe489002f
Source dataset
uspto-grants-1999_02
Patent number
US05874421

Reaction notes

Loading…