関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | tert-butyl N-(4-chlorophenyl)carbamate | HCID 546372 | — |
| 反応物 | Ethyl 2-(2,3-dimethoxyphenyl)-2-oxoacetate | HCID 21905960 | — |
| 反応物 | HCID 178418306 | HCID 178418306 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 21925471 | HCID 21925471 | — |
反応手順
A mixture of 11.4 g of tert-butyl 4-chlorophenylcarbamate in 100 ml of ether is cooled to −40° C., under an atmosphere of dry nitrogen, 80 ml of a 1.5M solution of tert-butyllithium in pentane are added dropwise and the mixture is stirred at −20° C. for 3 hours. The reaction mixture is cooled to −40° C., a solution of 14 g of the compound obtained in step A in 50 ml of THF is added over 1 hour, and the mixture is stirred at RT for 4 days. The reaction mixture is poured into saturated NH4Cl solution and the precipitate formed is filtered off by suction and dried. 10.2 g of the expected product are obtained, and are used without further purification in the following step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07119086B2 |
|---|
| 出典データセット | uspto-grants-2006_10 |
|---|
| ORD ID | ord-9fc61e64fc7149f489ae6c61e8b35d91 |
|---|
| 出典メモ | uspto-grants-2006_10 |
|---|
