Manganese(2+) dichloride → HCID 86750568, compound

HRID 976202Notes

Reaction equation

HRID 976202 reaction equation
[CH:1]1([CH:7]2[CH2:21][NH:20][CH2:19][CH2:18][NH:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][NH:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl-:22].[Mn+2:23].[Cl-:24]>CO>[Cl:22][C:7]1([CH:1]2[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2)[CH2:21][NH:20][CH2:19][CH2:18][NH:17][CH2:16][CH2:15][NH:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9][N:8]1[Cl:24].[Mn+2:23]

Participants

4

Reactant 2

HCID 10313134Manganese(2+) dichlorideHCID 18705607HCID 18705607, compound

Product 1

HCID 86750568HCID 86750568, compoundYield 62%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

2-Cyclohexyl-1,4,7,10,13-pentaazacyclopentadecane prepared as in Example 30E (0.50 g, 1.7 mmol) was added to a refluxing anhydrous MeOH solution (50 ml) containing anhydrous manganese(II) chloride (0.21 g, 1.7 mmol) under a dry nitrogen atmosphere. After refluxing for 2 h, the solution was stirred overnight at room temperature. The solution was filtered through celite and then taken to dryness. The solid was recrystallized from EtOH to give 0.44 g (62% yield) of a white solid after washing with ethyl ether and drying in vacuo: FAB mass spectrum (NBA+Li) m/z (relative intensity) 429 (M+ +Li, 5), 387/389 [(M+ -Cl), 100/35]; Anal. calcd for C16H35N5MnCl2 : C, 45.40; H, 8.33; N, 16.54; Cl, 16.75. Found: C, 45.39; H, 8.04; N, 16.33; C1, 16.37.

Workup

  1. temperatureAfter refluxing for 2 h
  2. filtrationThe solution was filtered through celite
  3. customThe solid was recrystallized from EtOH

Sources & evidence

ORD record
ord-cb9d6b975a0b49b6a2477f6f436b7da6
Source dataset
uspto-grants-1997_03
Patent number
US05610293

Reaction notes

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