Hydrogen Peroxide → HCID 178460128, Verbindung

HRID 2171324Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2171324
Cl[C:2]1[N:7]=[C:6]([N:8]([CH3:13])[CH:9]([CH3:12])[CH2:10][OH:11])[CH:5]=[C:4]([Cl:14])[N:3]=1.[Li+].[OH-:16].OO>O>[Cl:14][C:4]1[CH:5]=[C:6]([N:8]([CH:9]([CH3:12])[CH2:10][OH:11])[CH3:13])[NH:7][C:2](=[O:16])[N:3]=1

Komponenten

5

Edukt 3

HCID 784Hydrogen PeroxideHCID 3939Lithium HydroxideHCID 867283112-((2,6-Dichloropyrimidin-4-yl)(methyl)amino)propan-1-ol

Produkt 1

HCID 178460128HCID 178460128, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

To a mixture of 2-((2,6-dichloropyrimidin-4-yl)(methyl)amino)propan-1-ol (3.0 g, 13 mmol) and LiOH one hydrate (1.60 g, 38 mmol) in water (2 mL) was added H2O2 (0.78 mL, 25 mmol). The reaction mixture was stirred at 45° C. for 3 h, then quenched with Na2S3O3 solution (2 mL) and concentrated. Purification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3 in H2O/CH3CN, 10˜95%, 9.5 min, 30 mL/min) afforded the title product as a white solid.

Aufarbeitung

  1. customquenched with Na2S3O3 solution (2 mL)
  2. concentrationconcentrated
  3. customPurification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3 in H2O/CH3CN, 10˜95%, 9.5 min, 30 mL/min)

Quellen und Nachweise

ORD-Eintrag
ord-17d570f753b74906b0b84a76d556e440
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09051325B2

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