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Aluminum(III) Chloride → 6-(3-Carbomethoxy-2-methyl-propionyl)-3,4-dihydro-4-methyl-2(1H)-quinazolinone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 4-Methyl-3,4-dihydro-1H-quinazolin-2-one | HCID 12360757 | — |
| 反応物 | Methyl 4-chloro-3-methyl-4-oxobutanoate | HCID 14403282 | — |
| 溶媒 | Carbon Disulfide | HCID 6348 | — |
| 生成物 | 6-(3-Carbomethoxy-2-methyl-propionyl)-3,4-dihydro-4-methyl-2(1H)-quinazolinone | HCID 14620639 | — |
反応手順
3,4-Dihydro-4-methyl-2(1H)-quinazolinone (3.9 g) is added to a stirred suspension of anhydrous aluminum chloride (16.5 g) in carbon disulfide (120 ml) under nitrogen. 3-Carbomethoxy-2-methyl-propionyl chloride (4 g) is added dropwise to the stirred suspension, which is refluxed for about 17 hours and cooled to RT. The liquid phase is decanted and the residue is treated with ice/H2O (150 ml) and extracted with methylene chloride. The organic extract is dried, filtered, and concentrated in vacuo, affording the desired crude product as an oil, 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 | US04906630 |
| 出典データセット | uspto-grants-1990_03 |
| ORD ID | ord-2730bdabea554667994afa5299d55c2b |
| 出典メモ | uspto-grants-1990_03 |