関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Chlorobenzhydryl chloride | HCID 241584 | — |
| 反応物 | HCID 86703762 | HCID 86703762 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | HCID 86703761 | HCID 86703761 | 50% |
反応手順
A mixture of methyl 4-(azetidin-3-ylmethoxy)-5-cyclopropyl-2-fluorobenzoate (58 mg, 0.21 mmol), 1-chloro-4-(chloro(phenyl)methyl)benzene (74 mg, 0.31 mmol), potassium carbonate (86 mg, 0.62 mmol) and sodium iodide (32 mg, 0.21 mmol) in MeCN (10 mL) was stirred at 80° C. for 16 h. The reaction mixture was diluted with EtOAc (100 mL) and brine (50 mL). The organic layer was separated and washed with brine (50×2 mL), dried over anhydrous sodium sulfate, filtered and concentrated. The residue was purified by silica gel chromatography (eluting with petroleum ether/EtOAc=4/1) to give the target compound (50 mg, 50%) as a pale yellow oil. LCMS (ESI) m/z: 480.1 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08952169B2 |
|---|
| 出典データセット | uspto-grants-2015_02 |
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| ORD ID | ord-03ff19756b6c4eefb8063a25a595a1f7 |
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| 出典メモ | uspto-grants-2015_02 |
|---|
