関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | 1-Bromo-5-(1,1-dimethoxyethyl)-2-methoxy-3-trifluoromethylbenzene | HCID 58085697 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-[5-(1,1-Dimethoxyethyl)-2-methoxy-3-trifluoromethylphenyl]morpholine | HCID 58085699 | — |
反応手順
1-Bromo-5-(1,1-dimethoxyethyl)-2-methoxy-3-trifluoromethylbenzene (O3.004; 700 mg) was initially charged in dioxane (7 ml) and admixed successively with Pd(II) acetate (46 mg), cesium carbonate (2 g), 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene (118 mg) and morpholine (0.27 ml). Thereafter, the reaction mixture was heated to 90° C. for 7 h and then left to stand overnight. Subsequently, it was filtered and the filtrate was concentrated by rotary evaporation. The residue was purified using silica gel (50 g cartridge, n-heptane/EA gradient). 433 mg of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08198272B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-5907fae908c5441cb82e61b1e2545a83 |
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| 出典メモ | uspto-grants-2012_06 |
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