関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | O-Xylene | HCID 7237 | — |
| 反応物 | 1,2,3,6-Tetrahydropyridine | HCID 12750 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | HCID 178507684 | HCID 178507684 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178507852 | HCID 178507852 | — |
反応手順
155 G. of 2,4-diamino-6-chloropyrimidine-3-oxide are mixed and stirred under an argon atmosphere with 640 ml. of o-xylene and 260 ml. of 1,2,5,6-tetrahydropyridine. The mixture is then heated to reflux for 30 minutes, the internal temperature rising from 115° C. to 123° C. The mixture is then cooled to 5° C., treated with 40 g. of sodium hydroxide in 400 ml. of water and stirred at 5° C. for 1 hour. The precipitate formed is filtered off, washed with 200 ml. of water and recrystallized from 3000 ml. of water, there being obtained pure 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide having a melting point of 263°-265° C. (decomposition).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04150132 |
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| 出典データセット | uspto-grants-1979_04 |
|---|
| ORD ID | ord-67a44bf3e5c441a5bc8885e238cd2a91 |
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| 出典メモ | uspto-grants-1979_04 |
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