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Isopropenyl chloroformate → (3S)-6-Chloro-1-(isopropenyloxycarbonyl)-3-methyl-3,4-dihydro-1,4,5-triazanaphthalen-2(1H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropenyl chloroformate | HCID 93846 | — |
| 反応物 | (3S)-6-Chloro-3-methyl-3,4-dihydro-1,4,5-triazanaphthalen-2(1H)-one | HCID 57066600 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | (3S)-6-Chloro-1-(isopropenyloxycarbonyl)-3-methyl-3,4-dihydro-1,4,5-triazanaphthalen-2(1H)-one | HCID 57158666 | — |
反応手順
The compound of Example 2 (988 mg, 5.0 mmol) was dissolved in 30 ml of anhydrous pyridine. After addition of 0.6 ml (5.5 mmol) of isopropenyl chloroformate, the mixture was stirred at room temperature for 4 h and subsequently concentrated. The residue was dissolved in ethyl acetate and washed three times with water, dried (sodium sulfate) and concentrated. After chromatography on silica gel (ethyl acetate/heptane=1:2), the desired compound was isolated and crystallized from diethyl ether/pentane; yield 380 mg (27%) of melting point 86°-87° 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-6d6ed009073d40378300b3f99b4e6525 |
| 出典メモ | uspto-grants-1995_06 |