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 Trifluoroacetate | HCID 66879698 | — |
| 触媒 | Benzylidenebis(tricyclohexylphosphine)dichlororuthenium | HCID 11967259 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Trifluoroacetate | HCID 84468 | 66.9% |
| 生成物 | HCID 178478261 | HCID 178478261 | — |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08871753B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-7128b85503b74309844d0c1fc7a3dff8 |
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| 出典メモ | uspto-grants-2014_10 |
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