1-Methylpiperazine → [2-(4-Methylpiperazino)-5-nitrophenyl]methanol

HRID 1190863Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1190863
F[C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=1[CH2:4][OH:5].[CH3:13][N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>C1COCC1>[CH3:13][N:14]1[CH2:19][CH2:18][N:17]([C:2]2[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=2[CH2:4][OH:5])[CH2:16][CH2:15]1

Komponenten

4

Edukt 2

HCID 531671-MethylpiperazineHCID 4437169(2-Fluoro-5-nitrophenyl)methanol

Produkt 1

HCID 25918812[2-(4-Methylpiperazino)-5-nitrophenyl]methanolAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

2-Fluoro-5-nitrobenzyl alcohol (1 g, 5.84 mmol) and N-methylpiperazine (1.29 mL, 2 eq) were heated at 130° C. for 1 h. The reaction mixture was then diluted with 25 mL of THF and washed with a saturated aqueous solution of Na2CO3 and then with brine. The organic layer was dried over Na2SO4, filtered and evaporated. The residue was thoroughly washed with pentane and filtered off to yield expected compound as an orange powder (1.38 g, 94% yield). m/z (ESI) 252.1 [M+H]+.

Aufarbeitung

  1. washwashed with a saturated aqueous solution of Na2CO3
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. washThe residue was thoroughly washed with pentane
  6. filtrationfiltered off

Quellen und Nachweise

ORD-Eintrag
ord-a7a4d715d5a94319bcd29bd81c8f21d4
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08680095B2

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