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Carbon Disulfide → 6-(3-Carbomethoxy-3-methyl-propionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Disulfide | HCID 6348 | — |
| 反応物 | 3,4-Dihydro-3-methyl-2(1H)-quinazolinone | HCID 3846558 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | Methyl 4-chloro-3-methyl-4-oxobutanoate | HCID 14403282 | — |
| 生成物 | 6-(3-Carbomethoxy-3-methyl-propionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone | HCID 19863336 | — |
反応手順
3,4-Dihydro-3-methyl-2(1H)-quinazolinone (2.5 g) is added to a stirred suspension of anhydrous aluminum chloride (10.5 g) in carbon disulfide (120 ml) under nitrogen. 3-Carbomethoxy-2-methyl-propionyl chloride (2.5 g) is added dropwise to the stirred suspension, which is refluxed for about 18 hours and cooled to RT. The liquid phase is decanted and the residue treated with H2O (120 ml) and extracted with methylene chloride. The organic extract is dried, filtered and concentrated in vacuo, affording the desired product as a solid, which is used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04868300 |
| 出典データセット | uspto-grants-1989_09 |
| ORD ID | ord-d07d8f2ac7ab456da2be870ca14388dd |
| 出典メモ | uspto-grants-1989_09 |