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Tetrahydrofuran → HCID 18545432, Verbindung

HRID 1267085
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1267085
C1C[O:4][CH2:3]C1.Cl[C:7]1[N:12]=[C:11]([N:13]2[C:17]([CH3:18])=[C:16](/[CH:19]=[CH:20]/[CH2:21][N:22]3[CH2:27][CH2:26][N:25]([C:28]4[CH:33]=[C:32]([F:34])[CH:31]=[C:30]([F:35])[CH:29]=4)[CH2:24][CH2:23]3)[CH:15]=[N:14]2)[CH:10]=[C:9]([CH3:36])[N:8]=1.CO[C:39]1[CH:46]=[CH:45][C:42]([CH2:43][NH2:44])=[CH:41][CH:40]=1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)Cl>[F:35][C:30]1[CH:29]=[C:28]([N:25]2[CH2:26][CH2:27][N:22]([CH2:21]/[CH:20]=[CH:19]/[C:16]3[CH:15]=[N:14][N:13]([C:11]4[CH:10]=[C:9]([CH3:36])[N:8]=[C:7]([NH:44][CH2:43][C:42]5[CH:41]=[CH:40][CH:39]=[CH:46][C:45]=5[O:4][CH3:3])[N:12]=4)[C:17]=3[CH3:18])[CH2:23][CH2:24]2)[CH:33]=[C:32]([F:34])[CH:31]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 754524-MethoxybenzylamineHCID 18545346HCID 18545346, Verbindung

Produkt 1

HCID 18545432HCID 18545432, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212
Chloroform
Lösungsmittel

Versuchsvorschrift

To 15 ml of a THF solution of 155 mg of the compound obtained in Example 35 were added 240 mg of p-methoxybenzylamine and 50 mg (0.362 mmol) of potassium carbonate, followed by refluxing for 60 hours. Chloroform was added to the reaction mixture, and the mixture was washed with a saturated sodium chloride aqueous solution. The combined organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated. The residue was subjected to silica gel column chromatography using a 99:1 mixture (by volume) of chloroform and methanol as a developing solution. The fraction containing the desired compound was concentrated to give 183 mg of the title compound.

Aufarbeitung

  1. temperatureby refluxing for 60 hours
  2. washthe mixture was washed with a saturated sodium chloride aqueous solution
  3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated
  5. additionThe fraction containing the desired compound
  6. concentrationwas concentrated

Quellen und Nachweise

ORD-Eintrag
ord-1174ca4289e1479794b669403921b595
Quelldatensatz
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06552018B1

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