関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2-Chlorobenzaldehyde | HCID 6996 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | Methyl 4-(2-(1,3-dioxoisoindolin-2-yl)ethoxy)-3-oxobutanoate | HCID 22568398 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Methyl 2-(o-chlorobenzylidene)-4-(2-phthalimidoethoxy)acetoacetate | HCID 69267975 | — |
反応手順
85 g of methyl 4-(2-(phthalimido)ethoxy)acetoacetate was agitated with 31.7 ml of 2-chlorobenzaldehyde and 37 ml of 2-propanol at 20-25° C. The solution of 1.1 ml of piperidine in 14 ml of 2-propanol was added dropwise during 1.5 hour. The mixture was than agitated for 2 hours at the same temperature and for 2 hours at 35-40° C. The mixture was acidified with 1.5 ml of acetic acid, 140 ml of 2-propanol was added and the solution was cooled to 0-5° C. The isopropanolic layer was separated and the organic layer was again washed with 53 ml of 2-propanol. The organic layer, containing the desired product, was evaporated to dryness in order to remove the residual solvent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06858738B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-f4363df668ef423ea1801561f3f5fbda |
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| 出典メモ | uspto-grants-2005_02 |
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