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Ethanol → 2,3,8,9-Tetrahydro-5-(3,4,5-trimethoxyphenyl)-9-[(3,4,5-trimethoxyphenyl)methylene]-5H,6H-pyrano[4,3-d]thiazolo[3,2-a]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 4,5-Dihydro-2-thiazolamine | HCID 15689 | — |
| 反応物 | Tetrahydro-3,5-bis[(3,4,5-trimethoxyphenyl)methylene]-4H-pyran-4-one | HCID 2740872 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2,3,8,9-Tetrahydro-5-(3,4,5-trimethoxyphenyl)-9-[(3,4,5-trimethoxyphenyl)methylene]-5H,6H-pyrano[4,3-d]thiazolo[3,2-a]pyrimidine | HCID 21786680 | — |
反応手順
A stirred solution of tetrahydro-3,5-bis[(3,4,5-trimethoxyphenyl)methylene]-4H-pyran-4-one (3.0 g, 6.5 mmole) and 2-amino-2-thiazoline (0.8 g, 7.8 mmole) in 75 ml of CHCl3 is heated at reflux for 44 hours. After cooling, the solution is filtered to remove a small amount of insoluble material. The solvent is evaporated to give an oily residue which solidifies when treated with a small amount of EtOH. The yield is 2.2 g, m.p. 166°-168°. Crystallization from 10 ml of MeCN gives 1.5 g (42%) of light yellow solid, m.p. 153°-155°. The m.p. of a sample of this material does not change when recrystallized from MeCN.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04128648 |
| 出典データセット | uspto-grants-1978_12 |
| ORD ID | ord-21dd2336b8384ddb984830a2611bafb1 |
| 出典メモ | uspto-grants-1978_12 |