関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 反応物 | Ethyl 5-bromo-2-chlorobenzoate | HCID 144749 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-(4-Chloro-3-ethoxycarbonyl-phenyl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 53649170 | 97.2% |
反応手順
Piperazine-1-carboxylic acid tert-butyl ester (106 mg), 3-bromo-6-chlorobenzoic acid ethyl ester (125 mg), cesium carbonate (220 mg), palladium acetate (5 mg) and R-BINAP (22 mg) were combined in toluene (2 ml) and heated at 100° C. in a sealed vessel for 48 hr. The cooled reaction was loaded onto a silica column and eluted with iso-hexane/ethyl acetate (4:1) to give the subtitle product (170 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06555541B1 |
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| 出典データセット | uspto-grants-2003_04 |
|---|
| ORD ID | ord-f63c3d2e23c54986ae9032bf5396e921 |
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| 出典メモ | uspto-grants-2003_04 |
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