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HRID 541558Erstellt: 27. Oktober 2026

5-Chloro-N,N'-bis(3-vinylphenyl)pyrimidine-2,4-diamine Trifluoroacetate → Trifluoroacetate

https://huagongshe.com/reaction/541558

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
Edukt5-Chloro-N,N'-bis(3-vinylphenyl)pyrimidine-2,4-diamine TrifluoroacetateHCID 66879698—
KatalysatorBenzylidenebis(tricyclohexylphosphine)dichlororutheniumHCID 11967259—
Lösungsmittel1,2-DichloroethaneHCID 11—
LösungsmittelAcetonitrileHCID 6342—
ProduktTrifluoroacetateHCID 8446866,9%
ProduktHCID 178478261HCID 178478261—

Reaktionsbedingungen

Temperatur130 °C

Reaktionsschritte

A solution of 5-chloro-N,N′-bis(3-vinylphenyl)pyrimidine-2,4-diamine trifluoroacetate (21 mg, 0.045 mmol) in 1,2-dichloroethane (20 mL) was degassed by bubbling nitrogen for 5 minutes. Benzylidene-bis(tricyclohexylphosphine)dichlororuthenium (11 mg, 0.013 mmol) was added and the mixture was heated to 130° C. for 20 minutes in a microwave. The mixture was evaporated to give a dark mixture which was suspended in acetonitrile and filtered. The filtrate was purified by preparative LCMS (pH 2) to give the desired product as a trifluoroacetate salt (1.7 mg, 9%). LCMS for C18H14ClN4 (M+H)+: m/z=321.1. 1H NMR (400 MHz, CD3Cl): δ 8.85 (s, 1H), 8.75 (s, 1H), 7.90 (s, 1H), 7.55 (s, 1H), 7.25 (m, 3H), 7.02 (m, 4H), 6.60 (s, 2H).

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08871753B2
Quelldatensatzuspto-grants-2014_10
ORD IDord-7128b85503b74309844d0c1fc7a3dff8
Quellennotizuspto-grants-2014_10