関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 3-Morpholinone | HCID 66953 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | Methyl 4-bromo-3-nitrobenzoate | HCID 2736829 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Methyl 4-(morpholin-3-on-4-yl)-3-nitro-benzoate | HCID 67049467 | — |
反応手順
1.00 g (3.85 mmol) methyl 4-bromo-3-nitro-benzoate are dissolved in 6 ml dioxane with 389 mg (3.85 mmol) morpholin-3-one under a nitrogen atmosphere and 36.6 mg (40 μmol) tris-(dibenzylideneacetone)-dipalladium(0), 67.1 mg (116 μmol) xantphos and 1.75 g (5.38 mmol) caesium carbonate are added. Under a nitrogen atmosphere and with stirring, the reaction mixture is heated to 95° C. for 16 hours. Then it is filtered, the solution is evaporated down i. vac. and evaporated with ether. The residue is further reacted without any more purification. Yield: 1.31 g (quantitative).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07371743B2 |
|---|
| 出典データセット | uspto-grants-2008_05 |
|---|
| ORD ID | ord-1b04fe22a8e141d4ac95f0fdb3692797 |
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| 出典メモ | uspto-grants-2008_05 |
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