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Sodium sulfate decahydrate → [4-(6-aminomethyl-1-methyl-1H-benzimidazol-2-yl)-benzyl]-dipropyl-amine

HRID 2080796
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2080796
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:10]([CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[N:22]([CH3:32])[C:23]3[CH:29]=[C:28]([C:30]#[N:31])[CH:27]=[CH:26][C:24]=3[N:25]=2)=[CH:17][CH:16]=1)[CH2:11][CH2:12][CH3:13])[CH2:8][CH3:9].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[NH2:31][CH2:30][C:28]1[CH:27]=[CH:26][C:24]2[N:25]=[C:21]([C:18]3[CH:19]=[CH:20][C:15]([CH2:14][N:10]([CH2:7][CH2:8][CH3:9])[CH2:11][CH2:12][CH3:13])=[CH:16][CH:17]=3)[N:22]([CH3:32])[C:23]=2[CH:29]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 231553902-(4-dipropylaminomethyl-phenyl)-3-methyl-3H-benzimidazol-5-carbonitrile

Produkt 1

HCID 23155373[4-(6-aminomethyl-1-methyl-1H-benzimidazol-2-yl)-benzyl]-dipropyl-amineAusbeute 59,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028
Tetrahydrofuran
Lösungsmittel
2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Lithium aluminum hydride (64.0 mg) was suspended in THF (5.0 ml) and the whole was cooled to 0° C. A THF solution (5.0 ml) containing the compound (155 mg) obtained in Example 29-5 was dropped therein and the whole was stirred at 0° C. for 1 hour. After completion of the reaction, sodium sulfate decahydrate was added thereto until bubbling was stopped, and a 1 mol/l sodium hydroxide aqueous solution was then added thereto until a white precipitate was generated. A solid was separated by filtration and the solvent in the filtrate was then distillated off under reduced pressure, and the residue was dried under vacuum, thereby obtaining the subject compound (93.5 mg) as a yellow oily substance.

Aufarbeitung

  1. additionwas dropped
  2. additionwas added
  3. customuntil bubbling
  4. additiona 1 mol/l sodium hydroxide aqueous solution was then added
  5. customA solid was separated by filtration
  6. customthe residue was dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-74d36e780d684fe8b35c87cdbf385651
Quelldatensatz
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07932281B2

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