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Isopropenyl chloroformate → (2RS)-1-(Isopropenyloxycarbonyl)-2-methyl-1,2-dihydro-1,4,6-triazanaphthalen-3(4H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropenyl chloroformate | HCID 93846 | — |
| 反応物 | 2-methyl-1H,2H,3H,4H-pyrido[3,4-b]pyrazin-3-one | HCID 19932881 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | (2RS)-1-(Isopropenyloxycarbonyl)-2-methyl-1,2-dihydro-1,4,6-triazanaphthalen-3(4H)-one | HCID 19932849 | 12% |
反応手順
(2RS)-2-Methyl-1,2-dihydro-1,4,6-triazanaphthalen-3(4H)-one (A. Albert, G. B. Barlin J. Chem. Soc. 1963, 5156) (570 mg, 3.5 mmol) was dissolved in 30 ml of anhydrous pyridine and cooled in an ice bath. 0.42 ml (3.8 mmol) of isopropenyl chloroformate was added dropwise, and the mixture was subsequently stirred at room temperature overnight. Concentration, chromatography on silica gel (ethyl acetate/methanol=20:1) and crystallization (pentane/diethyl ether) resulted in 100 mg (12%) of the desired product of melting point 170°-171° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424311 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-51bf8dc81a7448649807c64ccbba7baf |
| 出典メモ | uspto-grants-1995_06 |