Hydrochloric Acid → Amino(1,4,5,6-tetrahydropyrimidine-5-yl)acetamide dihydrochloride

HRID 1681902Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1681902
[NH2:1][CH:2]([C:6]1[CH:7]=[N:8][CH:9]=[N:10][CH:11]=1)[C:3]([NH2:5])=[O:4].[ClH:12]>O>[ClH:12].[ClH:12].[NH2:1][CH:2]([CH:6]1[CH2:11][NH:10][CH:9]=[N:8][CH2:7]1)[C:3]([NH2:5])=[O:4]

Komponenten

4

Versuchsvorschrift

Amino(pyrimidin-5-yl)acetamide (950 mg, 6.7 mmol) is suspended in a mixture of 50 ml water and concentrated hydrochloric acid (13.3 mmol). The mixture is hydrogenated at 26 psig over 300 mg Pd-on-carbon 10% in a Parr hydrogenator for 3 h. Then the suspension is filtered and the filter rinsed twice with hot water (20 ml). The filtrate can be evaorated in vacuo to give 1.41 g yellow oil (92%). The oil is crystallized from anhydrous methanol/THF to give 1.33 g (87%) white crystals, identified by 300 MHz nmr.

Aufarbeitung

  1. filtrationThen the suspension is filtered
  2. washthe filter rinsed twice with hot water (20 ml)

Quellen und Nachweise

ORD-Eintrag
ord-13091bcb35a94d2185dc132fd1fadf16
Quelldatensatz
uspto-grants-1992_12
Patentnummer
US05175166

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