Manganese(2+) dichloride → HCID 86750566, compound

HRID 1683237Notes

Reaction equation

HRID 1683237 reaction equation
[CH2:1]([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)[C:2]#[CH:3].[Cl-:19].[Mn+2:20].[Cl-:21]>CO.C(O)C>[Cl:19][C:4]1([CH2:1][C:2]#[CH:3])[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:21].[Mn+2:20]

Participants

5

Reactant 2

HCID 10313134Manganese(2+) dichlorideHCID 18705619HCID 18705619, compound

Product 1

HCID 86750566HCID 86750566, compoundYield 80%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 887MethanolSolvent

Procedure

A solution of 2-propargyl-1,4,7,10,13-pentaazacyclopentadecane prepared as in Example 29G (310 mg, 1.22 mmol) and anhydrous manganese(II) chloride (154 mg, 1.22 mol) in methanol (50 ml) were refluxed under a dry nitrogen atmosphere for 2 h and then stirred overnight at room temperature. The solution was taken to dryness, redissolved in absolute ethanol (15 ml) and filtered through celite. Concentration and recrystallization from ethanol-ether afforded 370 mg (80% yield) of white microcrystalline product: FAB mass spectrum (NBA) m/z (relative intensity) 378 (M+, 2), 343/345 ((M-Cl)+, 100/30); Anal. calcd. for C13H27Cl2MnN5 : C, 41.14; H, 7.18; N, 18.47. Found: C, 40.49; H, 6.56; N, 18.14.

Workup

  1. temperaturewere refluxed under a dry nitrogen atmosphere for 2 h
  2. filtrationfiltered through celite
  3. concentrationConcentration and recrystallization from ethanol-ether

Sources & evidence

ORD record
ord-3835c7351e424d94ab5ea0ef10e1f46c
Source dataset
uspto-grants-1997_06
Patent number
US05637578

Reaction notes

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