関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Morpholinone | HCID 66953 | — |
| 反応物 | Benzyl(3-bromo-2-ethylphenyl)sulfane | HCID 66911124 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-(3-(Benzylthio)-2-ethylphenyl)morpholin-3-one | HCID 66911145 | — |
反応手順
Intermediate 4 (1.075 g, 3.5 mmol), morpholin-3-one (389 mg, 3.85 mmol), CuI (67 mg, 0.35 mmol), N,N′-dimethylethylene diamine (75 μl, 0.7 mmol) and K2CO3 (1.064 g, 7.7 mmol) were suspended in toluene (30 ml) under argon and heated to 110° C. for 20 h. After cooling to RT the reaction mixture was quenched by addition of 100 ml sat. aq. NH4Cl, 150 ml concentrated NH3 in water and 100 ml water and extracted three times with ethyl acetate. The organic layers were combined and washed with water and sat. aq. NaCl-solution, dried with MgSO4, filtered and evaporated to dryness. The resulting oil crystallizes upon standing and was triturated with n-heptane-MTBE (19:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08835653B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-7ec6910c258a42a1b1e945b9df3675f2 |
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| 出典メモ | uspto-grants-2014_09 |
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