تفاعل #450567

معادلة التفاعل

methanol

2-cyclohexylmethyl-1,4,7,10,13-pentaazacyclopentadecane

manganese(II) chloride

→

product

المردود 65.0%

Manganese(II)dichloro(2-Cyclohexylethyl-1,4,7,10,13-pentaazacyclopentadecane)

المردود 65.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed under a dry nitrogen atmosphere overnight
2. 2
   ترشيحThe solution was filtered
3. 3
   تركيزconcentrated in vacuo to a volume of 3 ml
4. 4
   workup.ADDITIONEthyl ether (20 ml) was added

الإجراء التجريبي

A solution of 2-cyclohexylmethyl-1,4,7,10,13-pentaazacyclopentadecane prepared as in Example 7A (0.43 g, 1.4 mmole) and anhydrous manganese(II) chloride (0.17 g, 1.4 mmole) in anhydrous methanol (30 ml) was refluxed under a dry nitrogen atmosphere overnight. The solution was filtered and concentrated in vacuo to a volume of 3 ml. Ethyl ether (20 ml) was added. Upon cooling to 0° C., 0.39 g (65% yield) of the product was obtained as a white solid: FAB mass spectrum (NBA) m/z (relative intensity) 401/403 [(M-Cl)+, 100/33]: Anal. Calcd. for C17H37Cl2MnN5 : C, 46.69; H, 8.53; N, 16.09. Found: C, 45.87; H, 8.40; N, 15.55.

المصدر