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Methyl Ethyl Ketone → 4-[4-[2-(1,3-Dioxolan-2-yl)ethyl]phenoxyacetyl]-5-methyl-2-phenyloxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Ethyl Ketone | HCID 6569 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Bromo-1-(5-methyl-2-phenyl-1,3-oxazol-4-yl)ethan-1-one | HCID 14913650 | — |
| 反応物 | 4-[2-(1,3-Dioxolan-2-yl)ethyl]phenol | HCID 18546139 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-[4-[2-(1,3-Dioxolan-2-yl)ethyl]phenoxyacetyl]-5-methyl-2-phenyloxazole | HCID 18546170 | 57% |
反応手順
A mixture of 4-bromoacetyl-5-methyl-2-phenyloxazole (2.60 g), 4-[2-(1,3-dioxolan-2-yl)ethyl]phenol (1.82 g), potassium carbonate (1.28 g) and 2-butanone (60 ml) was stirred for 20 hours at temperatures ranging from 70 to 80° C. The reaction mixture was poured into water. Resulting crystalline precipitate was collected by filtration, which was purified by means of a silica gel column chromatography. From the fractions eluted with chloroform-methanol (100:1, v/v), 4-[4-[2-(1,3-dioxolan-2-yl)ethyl]phenoxyacetyl]-5-methyl-2-phenyloxazole (2.08 g, 57%) was obtained. Recrystallization from dichloromethane-isopropyl ether gave colorless prisms, m.p.119-120° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06552058B1 |
| 出典データセット | uspto-grants-2003_04 |
| ORD ID | ord-b3a23b2106cd4ea080612e7f40de8e6c |
| 出典メモ | uspto-grants-2003_04 |