関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexachloroethane | HCID 6214 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 反応物 | 4-(1,3-Oxazol-5-yl)benzonitrile | HCID 2777271 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Water ethylacetate | HCID 22728543 | — |
| 生成物 | 4-(2-Chlorooxazol-5-yl)benzonitrile | HCID 68443558 | 82% |
反応手順
To a solution of 4-Oxazol-5-yl-benzonitrile (3 g, 17.65 mmol) in anhydrous THF (80 mL) at −78° C. under an argon atmosphere was slowly added a solution of LiHMDS (21.2 mL, 1 M in THF, 21.2 mmol). After 1 h at −78° C., solid hexachloroethane (6.275 g, 26.48 mmol) was added. The mixture was then stirred at −78° C. for 1 h and allowed to slowly warm to room temperature and stir for 3 h. The reaction was diluted with AcOEt/H2O (50 mL/15 mL). The organic layer was washed with brine, dried with MgSO4 and filtered. After removal of solvent the solid obtained was recrystallize from Hexane to give the title compound as a white solid (2.95 g, 82%). m.p.=144° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08080669B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-e78b697eaa13435da6d81b1c6f83a030 |
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| 出典メモ | uspto-grants-2011_12 |
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