Sodium Hydroxide → HCID 178488129, Verbindung

HRID 1655230Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1655230
[OH-].[Na+].Cl.Cl[CH2:5][C:6]1[C:11]([F:12])=[C:10]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)[CH:9]=[CH:8][N:7]=1.[CH3:19][O:20][C:21]1[CH:30]=[CH:29][C:24]2[NH:25][C:26]([SH:28])=[N:27][C:23]=2[CH:22]=1>C(O)C>[O:16]1[CH2:17][CH2:18][N:13]([C:10]2[CH:9]=[CH:8][N:7]=[C:6]([CH2:5][S:28][C:26]3[NH:25][C:24]4[CH:29]=[CH:30][C:21]([O:20][CH3:19])=[CH:22][C:23]=4[N:27]=3)[C:11]=2[F:12])[CH2:14][CH2:15]1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 197911192-Chloromethyl-3-fluoro-4-morpholinopyridine hydrochlorideHCID 178488140HCID 178488140, Verbindung

Produkt 1

HCID 178488129HCID 178488129, VerbindungAusbeute 74,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

5N NaOH (3.39 ml) was added dropwise to a stirred solution of 2-chloromethyl-3-fluoro-4-morpholinopyridine hydrochloride (2.06 g) and 5-methoxy-(1H)-benzimidazole-2-thiol (1.39 g) in ethanol (35 ml). After 3 hours excess solvent was removed and the residue treated with water (80 ml) and extracted with dichloromethane. The extracts were washed with water, dried (K2CO3), excess solvent removed and the residue crystallised from ethyl acetate to yield 2-(4-morpholino-3-fluoro-2-pyridylmethylthio)-5-methoxy-(1H)-benzimidazole (2.16 g) m.p. 121°-123°.

Aufarbeitung

  1. customAfter 3 hours excess solvent was removed
  2. additionthe residue treated with water (80 ml)
  3. extractionextracted with dichloromethane
  4. washThe extracts were washed with water
  5. dry with materialdried (K2CO3), excess solvent
  6. customremoved
  7. customthe residue crystallised from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-b6b5e8f4a10a43efaa1a534c3602f7ba
Quelldatensatz
uspto-grants-1993_10
Patentnummer
US05250527

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