Allylamine → HCID 20718717, Verbindung

HRID 1250621

Reaktionsgleichung

Reaktionsgleichung von HRID 1250621
[CH2:1]([NH2:4])[CH:2]=[CH2:3].Cl[C:6]1[N:7]=[C:8]([NH:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:9]2[S:14][CH:13]=[C:12]([CH3:15])[C:10]=2[N:11]=1>O>[CH2:1]([NH:4][C:6]1[N:7]=[C:8]([NH:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:9]2[S:14][CH:13]=[C:12]([CH3:15])[C:10]=2[N:11]=1)[CH:2]=[CH2:3]

Komponenten

4

Edukt 2

HCID 7853AllylamineHCID 183264882-Chloro-7-methyl-4-neopentylaminothieno[3,2-d]pyrimidine

Produkt 1

HCID 20718717HCID 20718717, VerbindungAusbeute 63,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

In 2.28 g (40.0 mmol) of allylamine was dissolved 250 mg (0.9 mmol) of 2-chloro-7-methyl-4-neopentylaminothieno[3,2-d]pyrimidine, and the resulting solution was heated in a sealed tube at 140° C. for 24 hours. After the reaction mixture was cooled, 100 ml of water was added thereto, followed by extraction with ethyl acetate (20 ml×3). The organic layer was washed with 20 ml of water and dried over anhydrous sodium sulfate, and then the solvent was distilled off. The residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4) to give 165 mg (yield: 61.3%) of the title compound.

Aufarbeitung

  1. temperatureAfter the reaction mixture was cooled
  2. extractionfollowed by extraction with ethyl acetate (20 ml×3)
  3. washThe organic layer was washed with 20 ml of water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4)

Quellen und Nachweise

ORD-Eintrag
ord-f7636c58f46944e68fb38628c3653a80
Quelldatensatz
uspto-grants-2002_01
Patentnummer
US06339089B2

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