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1,4,7,10,13-Pentaazacyclopentadecane → HCID 86750557, 화합물

HRID 363375
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HRID 363375 반응식
[NH:1]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11][NH:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[Cl-:16].[Mn+2:17].[Cl-:18]>CO>[Cl:16][CH:2]1[CH2:3][NH:4][CH2:5][CH2:6][NH:7][CH2:8][CH2:9][NH:10][CH2:11][CH2:12][NH:13][CH2:14][CH2:15][N:1]1[Cl:18].[Mn+2:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1201961,4,7,10,13-PentaazacyclopentadecaneHCID 10313134Manganese(2+) dichloride

생성물 1

HCID 86750557HCID 86750557, 화합물수율 88%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 1,4,7,10,13-pentaazacyclopentadecane prepared as in Example 1E (2.0 g, 9.3 mmole) and anhydrous manganese(II) chloride (1.2 g, 9.3 mmole) in anhydrous methanol (50 ml) was refluxed under a dry nitrogen atmosphere for 3 h. The solution was filtered and the solvent removed in vacuo. The resulting solid was recrystallized from ethanol-ethyl ether to give 2.79 g (88% yield) of the product as an off-white crystalline solid: FAB mass spectrum (NBA) m/z (relative intensity) 340 (M+, 2), 305/307 ((M-Cl)+ 100/45)); Anal. Calcd. for C10H25Cl2MnN5 : C, 35.17; H, 7.38; Cl, 20.76; N 20.60. Found: C, 34.95; H, 7.31; Cl, 20.49; N, 20.22.

후처리

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

출처 및 근거

ORD 기록
ord-9d9440cfada9443da38d1f6e3024759f
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05874421

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