関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Chloro-2-nitroanisole | HCID 81110 | — |
| 反応物 | Tert-butyl 3-oxopiperazine-1-carboxylate | HCID 3157178 | — |
| 試薬 | Cesium carbonate | HCID 10796 | — |
| 触媒 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Tert-butyl 4-(3-methoxy-4-nitrophenyl)-3-oxopiperazine-1-carboxylate | HCID 68591567 | 100.3% |
反応手順
A mixture of tert-butyl 3-oxopiperazine-1-carboxylate (1500 mg, 7.49 mmol), 4-chloro-2-methoxy-1-nitrobenzene (1405 mg, 7.49 mmol),cesium carbonate (3417 mg, 10.49 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (195 mg, 0.34 mmol) and TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM (174 mg, 0.19 mmol)was dried for 15 min under HV. Degassed dioxane (17 ml) was added and the resulting mixture was stirred at 90°C for 16 hours under inert atmosphere. Work-up and purification: see EN02378-07-02. tert-butyl 4-(3-methoxy-4-nitrophenyl)-3-oxopiperazine-1-carboxylate (2640 mg, 100 %) was isolated as an orange foam. FLA 02378-10-01: 1H NMR, LC-MS: OK.
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-ba7ec5906e7d4fb89a5c2ef7e7a905ac |
|---|
| 出典メモ | 750 AstraZeneca ELN dataset |
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