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HRID 541558作成日:2026年10月25日

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

https://huagongshe.com/reaction/541558

反応式

関与物質

役割名称HCID仕込み量
反応物5-Chloro-N,N'-bis(3-vinylphenyl)pyrimidine-2,4-diamine TrifluoroacetateHCID 66879698—
触媒Benzylidenebis(tricyclohexylphosphine)dichlororutheniumHCID 11967259—
溶媒1,2-DichloroethaneHCID 11—
溶媒AcetonitrileHCID 6342—
生成物TrifluoroacetateHCID 8446866.9%
生成物HCID 178478261HCID 178478261—

反応条件

温度130 °C

反応手順

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).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08871753B2
出典データセットuspto-grants-2014_10
ORD IDord-7128b85503b74309844d0c1fc7a3dff8
出典メモuspto-grants-2014_10