関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Sodium Cyanate | HCID 517096 | — |
| 反応物 | 2-(1-hydroxyethyl)-6-methylpyrazolo[1,5-c]quinazolin-5(6H)-one | HCID 12961608 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-[1-[(Aminocarbonyl)oxy]ethyl]-6-methylpyrazolo[1,5-c]quinazolin-5(6H)-one | HCID 12961607 | — |
反応手順
To a suspension of 3.7 g (0.0172 mole) of 2-(1-hydroxyethyl)-6-methylpyrazolo[1,5-c]quinazolin-5(6H)-one in 30 ml of benzene there is added 2.6 g (0.036 mole) of solid, 90% sodium cyanate followed by the dropwise addition of 3.1 ml (0.041 mole) of trifluoroacetic acid. The reaction mixture is stirred on a magnetic stirrer at approximately 120 revolutions per minute for 2 hours at room temperature. By the end of this time a gum separates. The reaction mixture is subsequently treated with 15 ml of water with increased stirring speed after which a solid (insoluble in either phase) forms. This is filtered, washed with water and air dried to give 2.9 g (60% direct yield), m.p. 216°-221°. The solid is twice crystallized from chloroform-methanol (1:1) to give 2.0 g of analytically pure material, m.p. 250°-252°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04128644 |
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| 出典データセット | uspto-grants-1978_12 |
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| ORD ID | ord-d6300e909cbf4732a7250d8e25bac2a8 |
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| 出典メモ | uspto-grants-1978_12 |
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