関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | {2-[4-Chloro-3-(trifluoromethyl)phenyl]-1,3-benzoxazol-6-yl}methanol | HCID 68453052 | — |
| 反応物 | HCID 178448254 | HCID 178448254 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | [2-(4-Isobutyl-3-trifluoromethyl-phenyl)-benzooxazol-6-yl]-methanol | HCID 68453276 | — |
反応手順
A mixture of [2-(4-chloro-3-trifluoromethyl-phenyl)-benzooxazol-6-yl]-methanol (1 eq) and Pd(PBut3)2 (0.05 eq) is treated with isobutyl zinc bromide in THF (0.5 M, 3 eq). The resulting mixture is heated at 100° C. in microwave for 30 minutes. The reaction mixture is diluted with aqueous HCl (5%) and extracted with EtOAc. The organic solution is washed with brine and dried over Na2SO4. After concentration, the residue is purified by flash column chromatography (30% EtOAc in hexane) to give the desired intermediate [2-(4-isobutyl-3-trifluoromethyl-phenyl)-benzooxazol-6-yl]-methanol. MS: (ES+): 350.1 (M+1)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07750021B2 |
|---|
| 出典データセット | uspto-grants-2010_07 |
|---|
| ORD ID | ord-c4438a5e2a234cd480f9e8ee590bbef9 |
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| 出典メモ | uspto-grants-2010_07 |
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