Tetrahydrofuran → HCID 86664952, Verbindung

HRID 74291Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 74291
Cl.[NH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]3[O:15][C:16]4[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=4[N:18]=3)=[CH:13][C:8]=2[N:7]=[C:6]1[CH3:23].[CH3:24][N:25]=[C:26]=[S:27].C(N(CC)CC)C.C1COCC1>O.C(Cl)(Cl)Cl>[O:15]1[C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[N:18]=[C:14]1[C:12]1[CH:11]=[CH:10][C:9]2[N:5]([CH2:4][CH2:3][NH:2][C:26](=[S:27])[NH:25][CH3:24])[C:6]([CH3:23])=[N:7][C:8]=2[CH:13]=1

Komponenten

7

Edukt 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 11167Methyl isothiocyanateHCID 674977031-(2-Aminoethyl)-5-(benzoxazol-2-yl)-2-methylbenzimidazole hydrochloride

Produkt 1

HCID 86664952HCID 86664952, VerbindungAusbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

1-(2-Aminoethyl)-5-(benzoxazol-2-yl)-2-methylbenzimidazole hydrochloride (see Working Example 56) (0.20 g, 0.6 mmol), methyl isothiocyanate (0.17 g, 0.6 mmol), triethylamine (0.13 g, 13 mmol) and THF (2 mL) were added together, and stirred for 1 hour at room temperature. After cooling, chloroform and water were added and extraction was carried out. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The solid obtained was separated by filtration and dried to yield the title compound (0.08 g, 40% yield) as white crystals.

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextraction
  3. customAfter the organic layer obtained
  4. dry with materialwas dried over anhydrous sodium sulfate, it
  5. filtrationwas filtered
  6. concentrationconcentrated
  7. customThe solid obtained
  8. customwas separated by filtration
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2a8d93b5a41341c3a3b0bf5871e0ab9f
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08829035B2

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