関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propofol | HCID 4943 | — |
| 反応物 | Bromochloromethane | HCID 6333 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(Chloromethoxy)-1,3-diisopropylbenzene | HCID 11253147 | 75% |
反応手順
A four-necked 500 mL round bottom flask was equipped with a mechanical stirrer, nitrogen inlet, condenser and thermometer. It was charged with 17.8 grams (0.10 moles) of 2,6-diisopropylphenol, 200 mL of THF, 8.0 grams (0.20 mole) of sodium hydroxide pellets, and 387 grams (3.0 moles, 194 mL) of bromochloromethane. The reaction mixture was heated to 64° C. and held for 2-3 hours until no more 2,6-diisopropylphenol was present as measured by GC. After cooling to 25° C., the suspension was filtered and the filter cake was washed with THF. The THF was removed by rotary evaporation and the resultant oil was distilled under vacuum (0-1 torr, b.p.=80° C.) to give 16.9 grams (0.074 moles, 75% yield) of O-chloromethyl 2,6-diisopropyl phenol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07534776B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-265a662102b3457fa7ab3fcabbc9d075 |
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| 出典メモ | uspto-grants-2009_05 |
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